Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Arjan Kleij' _publ_contact_author_address ; Research Group Kleij Institute of Chemical Research of Catalonia (ICIQ) Av. Paisos Catalans 16 Tarragona Tarragona 43007 SPAIN ; _publ_contact_author_email AKLEIJ@ICIQ.ES _publ_section_title ; Autocatalytic demetalation of a Zn(salphen) complex provoked by unprotected N-heterocycles ; loop_ _publ_author_name 'Arjan Kleij' 'Jordi Benet-Buchholz' 'Eduardo C. Escudero-Adan' # Attachment 'AWK221_0.cif' data_awk221_0 _database_code_depnum_ccdc_archive 'CCDC 658372' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 N4 O2 Zn' _chemical_formula_weight 686.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 32.9872(19) _cell_length_b 9.8259(6) _cell_length_c 23.0204(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7461.6(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8767 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 39.17 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.848602 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45014 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 39.87 _reflns_number_total 11013 _reflns_number_gt 9450 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+2.3282P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11013 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.655777(3) 0.605813(11) 0.5000 0.01079(3) Uani 1 2 d S . . C1 C 0.630782(19) 0.70501(6) 0.38228(2) 0.01147(9) Uani 1 1 d . . . O1 O 0.623486(14) 0.69178(5) 0.437398(19) 0.01428(8) Uani 1 1 d . . . N1 N 0.704931(17) 0.59657(6) 0.44292(2) 0.01201(8) Uani 1 1 d . . . N2 N 0.63324(3) 0.40970(8) 0.5000 0.01418(12) Uani 1 2 d S . . C2 C 0.598680(19) 0.74659(6) 0.34358(2) 0.01257(9) Uani 1 1 d . . . N3 N 0.58526(3) 0.25411(8) 0.5000 0.01587(13) Uani 1 2 d S . . C3 C 0.60691(2) 0.75895(7) 0.28499(2) 0.01452(10) Uani 1 1 d . . . H3 H 0.5853 0.7852 0.2601 0.017 Uiso 1 1 calc R . . C4 C 0.64531(2) 0.73525(7) 0.25943(2) 0.01382(9) Uani 1 1 d . . . C5 C 0.67606(2) 0.69878(7) 0.29645(2) 0.01392(10) Uani 1 1 d . . . H5 H 0.7024 0.6845 0.2810 0.017 Uiso 1 1 calc R . . C6 C 0.669844(19) 0.68166(6) 0.35702(2) 0.01224(9) Uani 1 1 d . . . C7 C 0.55593(2) 0.77237(7) 0.36770(3) 0.01527(10) Uani 1 1 d . . . C8 C 0.53951(2) 0.64186(9) 0.39604(4) 0.02477(14) Uani 1 1 d . . . H8A H 0.5114 0.6566 0.4084 0.037 Uiso 1 1 calc R . . H8B H 0.5562 0.6187 0.4299 0.037 Uiso 1 1 calc R . . H8C H 0.5405 0.5671 0.3679 0.037 Uiso 1 1 calc R . . C9 C 0.55714(2) 0.88835(8) 0.41243(3) 0.02038(12) Uani 1 1 d . . . H9A H 0.5675 0.9711 0.3939 0.031 Uiso 1 1 calc R . . H9B H 0.5750 0.8628 0.4447 0.031 Uiso 1 1 calc R . . H9C H 0.5297 0.9051 0.4272 0.031 Uiso 1 1 calc R . . C10 C 0.52594(3) 0.81357(12) 0.32002(3) 0.02995(19) Uani 1 1 d . . . H10A H 0.5356 0.8963 0.3007 0.045 Uiso 1 1 calc R . . H10B H 0.4993 0.8309 0.3374 0.045 Uiso 1 1 calc R . . H10C H 0.5237 0.7399 0.2915 0.045 Uiso 1 1 calc R . . C11 C 0.65008(2) 0.74930(7) 0.19355(3) 0.01641(11) Uani 1 1 d . . . C12 C 0.69277(3) 0.70988(9) 0.17350(3) 0.02306(14) Uani 1 1 d . . . H12A H 0.7127 0.7702 0.1918 0.035 Uiso 1 1 calc R . . H12B H 0.6946 0.7187 0.1312 0.035 Uiso 1 1 calc R . . H12C H 0.6984 0.6155 0.1847 0.035 Uiso 1 1 calc R . . C13 C 0.61949(3) 0.65481(9) 0.16313(3) 0.02320(14) Uani 1 1 d . . . H13A H 0.6235 0.5612 0.1767 0.035 Uiso 1 1 calc R . . H13B H 0.6237 0.6588 0.1210 0.035 Uiso 1 1 calc R . . H13C H 0.5918 0.6843 0.1723 0.035 Uiso 1 1 calc R . . C14 C 0.64186(3) 0.89700(8) 0.17520(3) 0.02644(16) Uani 1 1 d . . . H14A H 0.6149 0.9244 0.1886 0.040 Uiso 1 1 calc R . . H14B H 0.6431 0.9040 0.1328 0.040 Uiso 1 1 calc R . . H14C H 0.6623 0.9568 0.1925 0.040 Uiso 1 1 calc R . . C15 C 0.704486(19) 0.63489(7) 0.38898(2) 0.01277(9) Uani 1 1 d . . . H15A H 0.7295 0.6316 0.3687 0.015 Uiso 1 1 calc R . . C16 C 0.740481(18) 0.54628(6) 0.46919(2) 0.01173(9) Uani 1 1 d . . . C17 C 0.77364(2) 0.49172(7) 0.43938(3) 0.01472(10) Uani 1 1 d . . . H17A H 0.7736 0.4899 0.3981 0.018 Uiso 1 1 calc R . . C18 C 0.80665(2) 0.44007(7) 0.46975(3) 0.01531(10) Uani 1 1 d . . . H18A H 0.8293 0.4047 0.4492 0.018 Uiso 1 1 calc R . . C19 C 0.59365(3) 0.38785(9) 0.5000 0.01495(14) Uani 1 2 d S . . H19 H 0.5738 0.4577 0.5000 0.018 Uiso 1 2 calc SR . . C20 C 0.65104(3) 0.28253(11) 0.5000 0.01714(15) Uani 1 2 d S . . H20 H 0.6794 0.2654 0.5000 0.021 Uiso 1 2 calc SR . . C21 C 0.62161(3) 0.18552(10) 0.5000 0.01824(16) Uani 1 2 d S . . H21 H 0.6254 0.0897 0.5000 0.022 Uiso 1 2 calc SR . . C22 C 0.54489(4) 0.19448(14) 0.5000 0.0364(3) Uani 1 2 d S . . H22A H 0.5437 0.1209 0.5287 0.055 Uiso 0.50 1 calc PR A -1 H22B H 0.5389 0.1579 0.4613 0.055 Uiso 0.50 1 calc PR A -1 H22C H 0.5249 0.2645 0.5100 0.055 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01031(5) 0.01374(5) 0.00833(4) 0.000 0.000 -0.00088(3) C1 0.0124(2) 0.0128(2) 0.00923(18) -0.00038(15) -0.00051(15) -0.00082(17) O1 0.01294(19) 0.0213(2) 0.00857(15) 0.00157(14) 0.00032(12) 0.00123(15) N1 0.0108(2) 0.0153(2) 0.00993(17) 0.00031(14) -0.00026(14) 0.00047(15) N2 0.0150(3) 0.0146(3) 0.0130(3) 0.000 0.000 -0.0013(2) C2 0.0134(2) 0.0142(2) 0.01003(19) -0.00052(16) -0.00096(15) 0.00101(18) N3 0.0147(3) 0.0124(3) 0.0205(3) 0.000 0.000 -0.0005(2) C3 0.0175(3) 0.0164(2) 0.00965(19) -0.00040(17) -0.00171(17) 0.00233(19) C4 0.0178(3) 0.0147(2) 0.00890(18) 0.00017(16) -0.00016(16) 0.00088(19) C5 0.0152(3) 0.0168(2) 0.00977(19) 0.00044(17) 0.00097(16) 0.00023(19) C6 0.0129(2) 0.0148(2) 0.00904(18) 0.00032(16) 0.00006(15) -0.00010(18) C7 0.0130(3) 0.0196(3) 0.0133(2) -0.00021(18) -0.00153(17) 0.00247(19) C8 0.0153(3) 0.0234(3) 0.0355(4) 0.0027(3) 0.0020(3) -0.0031(2) C9 0.0193(3) 0.0213(3) 0.0205(3) -0.0042(2) 0.0042(2) 0.0027(2) C10 0.0190(3) 0.0524(6) 0.0183(3) 0.0013(3) -0.0038(2) 0.0139(3) C11 0.0228(3) 0.0172(3) 0.00919(19) 0.00006(18) 0.00016(18) 0.0018(2) C12 0.0251(3) 0.0316(4) 0.0125(2) 0.0007(2) 0.0044(2) 0.0016(3) C13 0.0274(4) 0.0286(4) 0.0136(2) -0.0059(2) -0.0015(2) -0.0005(3) C14 0.0441(5) 0.0201(3) 0.0151(3) 0.0046(2) 0.0020(3) 0.0050(3) C15 0.0121(2) 0.0159(2) 0.01041(19) 0.00019(17) 0.00065(15) -0.00001(18) C16 0.0108(2) 0.0133(2) 0.01110(18) -0.00028(16) 0.00007(15) 0.00052(17) C17 0.0143(2) 0.0166(2) 0.0133(2) -0.00149(18) 0.00133(17) 0.00251(19) C18 0.0131(3) 0.0152(2) 0.0176(2) -0.00129(18) 0.00121(17) 0.00288(19) C19 0.0155(4) 0.0123(3) 0.0171(3) 0.000 0.000 -0.0001(3) C20 0.0153(4) 0.0174(4) 0.0187(3) 0.000 0.000 0.0018(3) C21 0.0184(4) 0.0136(4) 0.0228(4) 0.000 0.000 0.0028(3) C22 0.0163(5) 0.0187(5) 0.0742(11) 0.000 0.000 -0.0044(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9812(5) 10_556 ? Zn1 O1 1.9812(5) . ? Zn1 N2 2.0654(8) . ? Zn1 N1 2.0890(5) 10_556 ? Zn1 N1 2.0890(5) . ? C1 O1 1.2980(7) . ? C1 C6 1.4322(9) . ? C1 C2 1.4430(8) . ? N1 C15 1.2975(8) . ? N1 C16 1.4089(8) . ? N2 C19 1.3234(13) . ? N2 C20 1.3806(13) . ? C2 C3 1.3810(8) . ? C2 C7 1.5366(9) . ? N3 C19 1.3430(12) . ? N3 C21 1.3756(13) . ? N3 C22 1.4549(15) . ? C3 C4 1.4161(9) . ? C4 C5 1.3725(9) . ? C4 C11 1.5310(8) . ? C5 C6 1.4193(8) . ? C6 C15 1.4348(9) . ? C7 C10 1.5322(10) . ? C7 C9 1.5365(10) . ? C7 C8 1.5374(11) . ? C11 C12 1.5316(11) . ? C11 C14 1.5357(10) . ? C11 C13 1.5396(11) . ? C16 C17 1.3981(9) . ? C16 C16 1.4187(11) 10_556 ? C17 C18 1.3899(9) . ? C18 C18 1.3928(13) 10_556 ? C20 C21 1.3604(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 93.34(3) 10_556 . ? O1 Zn1 N2 101.79(2) 10_556 . ? O1 Zn1 N2 101.79(2) . . ? O1 Zn1 N1 88.76(2) 10_556 10_556 ? O1 Zn1 N1 153.30(2) . 10_556 ? N2 Zn1 N1 103.82(2) . 10_556 ? O1 Zn1 N1 153.30(2) 10_556 . ? O1 Zn1 N1 88.76(2) . . ? N2 Zn1 N1 103.82(2) . . ? N1 Zn1 N1 77.96(3) 10_556 . ? O1 C1 C6 123.21(5) . . ? O1 C1 C2 119.73(5) . . ? C6 C1 C2 117.06(5) . . ? C1 O1 Zn1 130.85(4) . . ? C15 N1 C16 121.46(5) . . ? C15 N1 Zn1 125.49(4) . . ? C16 N1 Zn1 113.04(4) . . ? C19 N2 C20 105.83(8) . . ? C19 N2 Zn1 120.43(6) . . ? C20 N2 Zn1 133.74(7) . . ? C3 C2 C1 118.92(6) . . ? C3 C2 C7 121.25(5) . . ? C1 C2 C7 119.80(5) . . ? C19 N3 C21 107.44(8) . . ? C19 N3 C22 125.65(9) . . ? C21 N3 C22 126.91(9) . . ? C2 C3 C4 124.55(6) . . ? C5 C4 C3 116.49(5) . . ? C5 C4 C11 124.24(6) . . ? C3 C4 C11 119.26(6) . . ? C4 C5 C6 122.28(6) . . ? C5 C6 C1 120.66(5) . . ? C5 C6 C15 115.25(5) . . ? C1 C6 C15 124.03(5) . . ? C10 C7 C9 107.51(7) . . ? C10 C7 C2 112.17(5) . . ? C9 C7 C2 109.91(6) . . ? C10 C7 C8 107.27(7) . . ? C9 C7 C8 110.08(6) . . ? C2 C7 C8 109.83(6) . . ? C4 C11 C12 111.72(6) . . ? C4 C11 C14 109.85(6) . . ? C12 C11 C14 108.57(7) . . ? C4 C11 C13 109.20(6) . . ? C12 C11 C13 108.24(6) . . ? C14 C11 C13 109.21(7) . . ? N1 C15 C6 126.35(6) . . ? C17 C16 N1 125.11(5) . . ? C17 C16 C16 119.40(3) . 10_556 ? N1 C16 C16 115.41(3) . 10_556 ? C18 C17 C16 120.41(5) . . ? C17 C18 C18 120.19(4) . 10_556 ? N2 C19 N3 111.23(8) . . ? C21 C20 N2 109.31(9) . . ? C20 C21 N3 106.18(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 O1 Zn1 -13.69(9) . . . . ? C2 C1 O1 Zn1 167.03(4) . . . . ? O1 Zn1 O1 C1 165.17(5) 10_556 . . . ? N2 Zn1 O1 C1 -92.05(6) . . . . ? N1 Zn1 O1 C1 71.29(8) 10_556 . . . ? N1 Zn1 O1 C1 11.81(6) . . . . ? O1 Zn1 N1 C15 -97.48(7) 10_556 . . . ? O1 Zn1 N1 C15 -2.52(6) . . . . ? N2 Zn1 N1 C15 99.31(6) . . . . ? N1 Zn1 N1 C15 -159.21(5) 10_556 . . . ? O1 Zn1 N1 C16 81.00(6) 10_556 . . . ? O1 Zn1 N1 C16 175.96(4) . . . . ? N2 Zn1 N1 C16 -82.21(4) . . . . ? N1 Zn1 N1 C16 19.27(5) 10_556 . . . ? O1 Zn1 N2 C19 47.991(14) 10_556 . . . ? O1 Zn1 N2 C19 -47.994(14) . . . . ? N1 Zn1 N2 C19 139.626(15) 10_556 . . . ? N1 Zn1 N2 C19 -139.627(15) . . . . ? O1 Zn1 N2 C20 -132.009(14) 10_556 . . . ? O1 Zn1 N2 C20 132.006(15) . . . . ? N1 Zn1 N2 C20 -40.374(16) 10_556 . . . ? N1 Zn1 N2 C20 40.373(15) . . . . ? O1 C1 C2 C3 -179.43(6) . . . . ? C6 C1 C2 C3 1.24(9) . . . . ? O1 C1 C2 C7 -1.12(9) . . . . ? C6 C1 C2 C7 179.56(6) . . . . ? C1 C2 C3 C4 -0.87(10) . . . . ? C7 C2 C3 C4 -179.16(6) . . . . ? C2 C3 C4 C5 -0.62(10) . . . . ? C2 C3 C4 C11 178.54(6) . . . . ? C3 C4 C5 C6 1.72(10) . . . . ? C11 C4 C5 C6 -177.39(6) . . . . ? C4 C5 C6 C1 -1.34(10) . . . . ? C4 C5 C6 C15 176.14(6) . . . . ? O1 C1 C6 C5 -179.51(6) . . . . ? C2 C1 C6 C5 -0.21(9) . . . . ? O1 C1 C6 C15 3.24(10) . . . . ? C2 C1 C6 C15 -177.46(6) . . . . ? C3 C2 C7 C10 -0.91(10) . . . . ? C1 C2 C7 C10 -179.18(7) . . . . ? C3 C2 C7 C9 -120.46(7) . . . . ? C1 C2 C7 C9 61.27(8) . . . . ? C3 C2 C7 C8 118.29(7) . . . . ? C1 C2 C7 C8 -59.98(8) . . . . ? C5 C4 C11 C12 3.22(10) . . . . ? C3 C4 C11 C12 -175.87(6) . . . . ? C5 C4 C11 C14 -117.33(8) . . . . ? C3 C4 C11 C14 63.58(9) . . . . ? C5 C4 C11 C13 122.93(7) . . . . ? C3 C4 C11 C13 -56.16(8) . . . . ? C16 N1 C15 C6 176.97(6) . . . . ? Zn1 N1 C15 C6 -4.68(10) . . . . ? C5 C6 C15 N1 -171.24(6) . . . . ? C1 C6 C15 N1 6.15(11) . . . . ? C15 N1 C16 C17 -21.43(10) . . . . ? Zn1 N1 C16 C17 160.03(5) . . . . ? C15 N1 C16 C16 162.05(5) . . . 10_556 ? Zn1 N1 C16 C16 -16.50(4) . . . 10_556 ? N1 C16 C17 C18 -177.52(6) . . . . ? C16 C16 C17 C18 -1.13(8) 10_556 . . . ? C16 C17 C18 C18 1.13(8) . . . 10_556 ? C20 N2 C19 N3 0.0 . . . . ? Zn1 N2 C19 N3 180.0 . . . . ? C21 N3 C19 N2 0.0 . . . . ? C22 N3 C19 N2 180.0 . . . . ? C19 N2 C20 C21 0.0 . . . . ? Zn1 N2 C20 C21 180.0 . . . . ? N2 C20 C21 N3 0.0 . . . . ? C19 N3 C21 C20 0.0 . . . . ? C22 N3 C21 C20 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 39.87 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.834 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.071 data_akw05_0m _database_code_depnum_ccdc_archive 'CCDC 658373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H54 N4 O2 Zn' _chemical_formula_weight 736.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4787(6) _cell_length_b 14.6726(11) _cell_length_c 14.9753(10) _cell_angle_alpha 103.503(4) _cell_angle_beta 107.774(3) _cell_angle_gamma 91.800(4) _cell_volume 1916.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7531 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.843338 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37644 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 39.97 _reflns_number_total 16419 _reflns_number_gt 14327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.3096P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16419 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.655090(10) 0.300299(8) 0.039872(6) 0.00945(3) Uani 1 1 d . . . O1 O 0.85977(7) 0.30344(6) 0.12657(4) 0.01274(14) Uani 1 1 d . . . N1 N 0.62561(7) 0.41368(6) 0.14351(5) 0.01058(14) Uani 1 1 d . . . C1 C 0.94074(8) 0.36573(7) 0.20402(5) 0.01070(16) Uani 1 1 d . . . O2 O 0.69773(7) 0.24860(6) -0.08271(4) 0.01300(14) Uani 1 1 d . . . N2 N 0.46346(7) 0.35109(6) -0.03989(5) 0.01038(14) Uani 1 1 d . . . C2 C 1.09673(8) 0.35541(7) 0.24661(5) 0.01038(16) Uani 1 1 d . . . N3 N 0.54340(8) 0.18619(7) 0.06125(5) 0.01300(15) Uani 1 1 d . . . C3 C 1.18101(9) 0.42406(8) 0.32815(6) 0.01180(17) Uani 1 1 d . . . H3A H 1.2836 0.4173 0.3549 0.014 Uiso 1 1 calc R . . N4 N 0.37122(8) 0.06477(7) 0.02806(5) 0.01394(16) Uani 1 1 d . . . C4 C 1.12552(9) 0.50334(8) 0.37439(5) 0.01172(17) Uani 1 1 d . . . C5 C 0.97724(9) 0.51231(8) 0.33406(6) 0.01192(17) Uani 1 1 d . . . H5A H 0.9363 0.5653 0.3627 0.014 Uiso 1 1 calc R . . C6 C 0.88337(9) 0.44473(7) 0.25085(5) 0.01100(16) Uani 1 1 d . . . C7 C 0.73162(9) 0.46456(7) 0.21785(5) 0.01122(16) Uani 1 1 d . . . H7A H 0.7062 0.5203 0.2538 0.013 Uiso 1 1 calc R . . C8 C 0.48365(8) 0.44575(7) 0.11689(5) 0.00997(16) Uani 1 1 d . . . C9 C 0.42531(9) 0.50354(8) 0.18185(6) 0.01274(17) Uani 1 1 d . . . H9A H 0.4789 0.5199 0.2493 0.015 Uiso 1 1 calc R . . C10 C 0.28898(9) 0.53727(8) 0.14815(6) 0.01454(18) Uani 1 1 d . . . H10A H 0.2496 0.5767 0.1926 0.017 Uiso 1 1 calc R . . C11 C 0.20977(9) 0.51333(8) 0.04907(6) 0.01434(18) Uani 1 1 d . . . H11A H 0.1195 0.5396 0.0258 0.017 Uiso 1 1 calc R . . C12 C 0.26243(9) 0.45144(8) -0.01537(6) 0.01230(17) Uani 1 1 d . . . H12A H 0.2061 0.4334 -0.0824 0.015 Uiso 1 1 calc R . . C13 C 0.39832(8) 0.41519(7) 0.01767(5) 0.00995(16) Uani 1 1 d . . . C14 C 0.40023(9) 0.31883(7) -0.13257(5) 0.01149(17) Uani 1 1 d . . . H14A H 0.3036 0.3361 -0.1596 0.014 Uiso 1 1 calc R . . C15 C 0.46237(9) 0.25940(7) -0.19829(5) 0.01115(16) Uani 1 1 d . . . C16 C 0.36941(9) 0.23432(8) -0.29590(5) 0.01287(17) Uani 1 1 d . . . H16A H 0.2698 0.2499 -0.3106 0.015 Uiso 1 1 calc R . . C17 C 0.41724(9) 0.18820(8) -0.37067(5) 0.01214(17) Uani 1 1 d . . . C18 C 0.56824(9) 0.17086(8) -0.34511(5) 0.01226(17) Uani 1 1 d . . . H18A H 0.6049 0.1414 -0.3959 0.015 Uiso 1 1 calc R . . C19 C 0.66729(9) 0.19392(7) -0.25062(5) 0.01095(16) Uani 1 1 d . . . C20 C 0.61244(8) 0.23477(7) -0.17214(5) 0.01032(16) Uani 1 1 d . . . C21 C 1.16459(9) 0.27090(7) 0.20040(6) 0.01153(17) Uani 1 1 d . . . C22 C 1.08426(10) 0.17747(8) 0.19965(6) 0.01511(18) Uani 1 1 d . . . H22A H 1.0897 0.1773 0.2660 0.023 Uiso 1 1 calc R . . H22B H 1.1325 0.1245 0.1732 0.023 Uiso 1 1 calc R . . H22C H 0.9796 0.1713 0.1593 0.023 Uiso 1 1 calc R . . C23 C 1.15037(10) 0.27203(8) 0.09542(6) 0.01582(19) Uani 1 1 d . . . H23A H 1.1945 0.2181 0.0665 0.024 Uiso 1 1 calc R . . H23B H 1.2027 0.3307 0.0955 0.024 Uiso 1 1 calc R . . H23C H 1.0448 0.2679 0.0575 0.024 Uiso 1 1 calc R . . C24 C 1.33104(10) 0.27277(9) 0.25595(7) 0.0169(2) Uani 1 1 d . . . H24A H 1.3434 0.2725 0.3233 0.025 Uiso 1 1 calc R . . H24B H 1.3861 0.3299 0.2548 0.025 Uiso 1 1 calc R . . H24C H 1.3697 0.2171 0.2251 0.025 Uiso 1 1 calc R . . C25 C 1.22914(9) 0.57594(8) 0.46327(6) 0.01326(18) Uani 1 1 d . . . C26 C 1.34257(11) 0.62783(9) 0.43216(7) 0.0196(2) Uani 1 1 d . . . H26A H 1.3988 0.5820 0.4026 0.029 Uiso 1 1 calc R . . H26B H 1.4114 0.6729 0.4891 0.029 Uiso 1 1 calc R . . H26C H 1.2896 0.6616 0.3850 0.029 Uiso 1 1 calc R . . C27 C 1.31310(10) 0.52567(9) 0.54004(6) 0.0180(2) Uani 1 1 d . . . H27A H 1.3756 0.4824 0.5135 0.027 Uiso 1 1 calc R . . H27B H 1.2410 0.4900 0.5576 0.027 Uiso 1 1 calc R . . H27C H 1.3761 0.5726 0.5979 0.027 Uiso 1 1 calc R . . C28 C 1.14439(11) 0.64911(10) 0.51017(7) 0.0213(2) Uani 1 1 d . . . H28A H 1.2151 0.6944 0.5660 0.032 Uiso 1 1 calc R . . H28B H 1.0733 0.6174 0.5318 0.032 Uiso 1 1 calc R . . H28C H 1.0905 0.6824 0.4628 0.032 Uiso 1 1 calc R . . C29 C 0.30854(10) 0.16202(8) -0.47489(6) 0.01419(18) Uani 1 1 d . . . C30 C 0.24539(11) 0.25146(9) -0.50053(6) 0.0203(2) Uani 1 1 d . . . H30A H 0.1740 0.2346 -0.5664 0.030 Uiso 1 1 calc R . . H30B H 0.3270 0.2963 -0.4969 0.030 Uiso 1 1 calc R . . H30C H 0.1949 0.2804 -0.4545 0.030 Uiso 1 1 calc R . . C31 C 0.17876(12) 0.09141(10) -0.48250(7) 0.0226(2) Uani 1 1 d . . . H31A H 0.1290 0.1193 -0.4357 0.034 Uiso 1 1 calc R . . H31B H 0.2176 0.0335 -0.4683 0.034 Uiso 1 1 calc R . . H31C H 0.1072 0.0766 -0.5483 0.034 Uiso 1 1 calc R . . C32 C 0.38356(11) 0.11667(9) -0.54909(6) 0.0171(2) Uani 1 1 d . . . H32A H 0.4234 0.0592 -0.5340 0.026 Uiso 1 1 calc R . . H32B H 0.4650 0.1611 -0.5464 0.026 Uiso 1 1 calc R . . H32C H 0.3102 0.1007 -0.6143 0.026 Uiso 1 1 calc R . . C33 C 0.83304(9) 0.17716(8) -0.22964(6) 0.01238(17) Uani 1 1 d . . . C34 C 0.87080(11) 0.13881(9) -0.32314(7) 0.0198(2) Uani 1 1 d . . . H34A H 0.9767 0.1295 -0.3067 0.030 Uiso 1 1 calc R . . H34B H 0.8496 0.1840 -0.3632 0.030 Uiso 1 1 calc R . . H34C H 0.8102 0.0785 -0.3592 0.030 Uiso 1 1 calc R . . C35 C 0.87383(11) 0.10526(9) -0.16818(7) 0.0191(2) Uani 1 1 d . . . H35A H 0.8143 0.0445 -0.2039 0.029 Uiso 1 1 calc R . . H35B H 0.8532 0.1281 -0.1070 0.029 Uiso 1 1 calc R . . H35C H 0.9800 0.0974 -0.1545 0.029 Uiso 1 1 calc R . . C36 C 0.93423(10) 0.27042(8) -0.17542(7) 0.01590(19) Uani 1 1 d . . . H36A H 0.9132 0.2975 -0.1151 0.024 Uiso 1 1 calc R . . H36B H 0.9149 0.3148 -0.2164 0.024 Uiso 1 1 calc R . . H36C H 1.0389 0.2583 -0.1602 0.024 Uiso 1 1 calc R . . C37 C 0.41905(9) 0.13685(8) -0.00145(6) 0.01395(18) Uani 1 1 d . . . H37A H 0.3683 0.1507 -0.0613 0.017 Uiso 1 1 calc R . . C38 C 0.47308(10) 0.06653(8) 0.11749(6) 0.01348(17) Uani 1 1 d . . . C39 C 0.48190(12) 0.00729(9) 0.17922(7) 0.0201(2) Uani 1 1 d . . . H39A H 0.4097 -0.0452 0.1638 0.024 Uiso 1 1 calc R . . C40 C 0.60205(13) 0.02937(10) 0.26438(8) 0.0251(2) Uani 1 1 d . . . H40A H 0.6131 -0.0092 0.3084 0.030 Uiso 1 1 calc R . . C41 C 0.70816(13) 0.10781(10) 0.28697(7) 0.0230(2) Uani 1 1 d . . . H41A H 0.7880 0.1213 0.3465 0.028 Uiso 1 1 calc R . . C42 C 0.69947(10) 0.16583(8) 0.22482(6) 0.0169(2) Uani 1 1 d . . . H42A H 0.7716 0.2184 0.2405 0.020 Uiso 1 1 calc R . . C43 C 0.57981(9) 0.14353(8) 0.13811(6) 0.01255(17) Uani 1 1 d . . . C44 C 0.23386(10) 0.00069(9) -0.02186(7) 0.0191(2) Uani 1 1 d . . . H44A H 0.1558 0.0234 0.0053 0.029 Uiso 1 1 calc R . . H44B H 0.2518 -0.0626 -0.0132 0.029 Uiso 1 1 calc R . . H44C H 0.2019 -0.0017 -0.0912 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.00891(4) 0.00997(7) 0.00880(4) 0.00147(3) 0.00256(3) 0.00113(3) O1 0.0107(2) 0.0117(4) 0.0118(2) -0.0014(2) 0.00102(18) 0.0018(2) N1 0.0090(2) 0.0117(5) 0.0104(2) 0.0019(2) 0.00281(19) 0.0025(2) C1 0.0096(3) 0.0115(5) 0.0103(3) 0.0018(3) 0.0029(2) 0.0003(3) O2 0.0115(2) 0.0178(4) 0.0087(2) 0.0019(2) 0.00271(17) 0.0031(2) N2 0.0103(2) 0.0108(5) 0.0099(2) 0.0017(2) 0.00375(19) 0.0011(3) C2 0.0099(3) 0.0100(5) 0.0107(3) 0.0017(3) 0.0033(2) 0.0016(3) N3 0.0128(3) 0.0130(5) 0.0141(3) 0.0043(3) 0.0049(2) 0.0011(3) C3 0.0094(3) 0.0122(5) 0.0124(3) 0.0017(3) 0.0025(2) 0.0015(3) N4 0.0129(3) 0.0110(5) 0.0180(3) 0.0024(3) 0.0060(2) 0.0007(3) C4 0.0104(3) 0.0113(5) 0.0114(3) 0.0003(3) 0.0025(2) 0.0003(3) C5 0.0108(3) 0.0112(6) 0.0116(3) -0.0001(3) 0.0027(2) 0.0020(3) C6 0.0098(3) 0.0114(5) 0.0102(3) 0.0006(3) 0.0025(2) 0.0014(3) C7 0.0105(3) 0.0114(5) 0.0109(3) 0.0012(3) 0.0033(2) 0.0025(3) C8 0.0092(3) 0.0099(5) 0.0110(3) 0.0023(3) 0.0036(2) 0.0017(3) C9 0.0121(3) 0.0133(6) 0.0125(3) 0.0011(3) 0.0051(2) 0.0026(3) C10 0.0126(3) 0.0140(6) 0.0169(3) 0.0011(3) 0.0063(3) 0.0038(3) C11 0.0104(3) 0.0140(6) 0.0183(3) 0.0035(3) 0.0045(2) 0.0035(3) C12 0.0100(3) 0.0128(6) 0.0136(3) 0.0033(3) 0.0030(2) 0.0018(3) C13 0.0091(3) 0.0104(5) 0.0106(3) 0.0026(3) 0.0036(2) 0.0011(3) C14 0.0103(3) 0.0131(5) 0.0105(3) 0.0023(3) 0.0029(2) 0.0017(3) C15 0.0110(3) 0.0119(5) 0.0098(3) 0.0015(3) 0.0033(2) 0.0010(3) C16 0.0120(3) 0.0145(6) 0.0103(3) 0.0014(3) 0.0024(2) 0.0013(3) C17 0.0134(3) 0.0117(5) 0.0098(3) 0.0014(3) 0.0025(2) 0.0007(3) C18 0.0142(3) 0.0119(5) 0.0101(3) 0.0012(3) 0.0042(2) 0.0011(3) C19 0.0118(3) 0.0099(5) 0.0110(3) 0.0018(3) 0.0042(2) 0.0013(3) C20 0.0108(3) 0.0100(5) 0.0100(2) 0.0020(3) 0.0034(2) 0.0008(3) C21 0.0109(3) 0.0115(5) 0.0118(3) 0.0016(3) 0.0040(2) 0.0020(3) C22 0.0170(3) 0.0105(6) 0.0174(3) 0.0030(3) 0.0052(3) 0.0026(3) C23 0.0178(3) 0.0177(6) 0.0134(3) 0.0028(3) 0.0078(3) 0.0034(3) C24 0.0116(3) 0.0173(7) 0.0191(3) 0.0006(3) 0.0039(3) 0.0041(3) C25 0.0115(3) 0.0119(6) 0.0129(3) -0.0011(3) 0.0022(2) -0.0003(3) C26 0.0172(4) 0.0172(7) 0.0219(4) 0.0035(4) 0.0044(3) -0.0037(4) C27 0.0176(3) 0.0196(7) 0.0128(3) 0.0021(3) 0.0009(3) 0.0008(4) C28 0.0169(4) 0.0184(7) 0.0198(4) -0.0069(4) 0.0022(3) 0.0027(4) C29 0.0150(3) 0.0153(6) 0.0097(3) 0.0006(3) 0.0022(2) 0.0010(3) C30 0.0221(4) 0.0230(7) 0.0135(3) 0.0041(3) 0.0025(3) 0.0083(4) C31 0.0212(4) 0.0254(8) 0.0156(3) -0.0014(4) 0.0037(3) -0.0065(4) C32 0.0204(4) 0.0179(6) 0.0111(3) 0.0011(3) 0.0040(3) 0.0046(4) C33 0.0122(3) 0.0116(5) 0.0135(3) 0.0017(3) 0.0054(2) 0.0025(3) C34 0.0176(4) 0.0250(7) 0.0168(3) 0.0005(3) 0.0089(3) 0.0057(4) C35 0.0182(4) 0.0174(7) 0.0250(4) 0.0091(4) 0.0082(3) 0.0068(4) C36 0.0124(3) 0.0137(6) 0.0205(3) 0.0011(3) 0.0061(3) 0.0009(3) C37 0.0131(3) 0.0129(6) 0.0163(3) 0.0041(3) 0.0051(2) 0.0021(3) C38 0.0150(3) 0.0106(6) 0.0166(3) 0.0030(3) 0.0078(3) 0.0019(3) C39 0.0242(4) 0.0161(7) 0.0242(4) 0.0090(4) 0.0110(3) 0.0013(4) C40 0.0324(5) 0.0236(7) 0.0234(4) 0.0137(4) 0.0090(4) 0.0020(5) C41 0.0271(4) 0.0243(7) 0.0177(4) 0.0097(4) 0.0044(3) 0.0011(4) C42 0.0184(4) 0.0174(6) 0.0147(3) 0.0048(3) 0.0046(3) 0.0004(4) C43 0.0139(3) 0.0109(5) 0.0142(3) 0.0032(3) 0.0065(2) 0.0018(3) C44 0.0144(3) 0.0138(7) 0.0264(4) 0.0007(4) 0.0064(3) -0.0017(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9699(6) . ? Zn1 O2 1.9825(6) . ? Zn1 N1 2.0839(8) . ? Zn1 N3 2.0910(8) . ? Zn1 N2 2.1113(8) . ? O1 C1 1.2988(10) . ? N1 C7 1.2993(11) . ? N1 C8 1.4110(12) . ? C1 C6 1.4227(14) . ? C1 C2 1.4489(12) . ? O2 C20 1.3001(9) . ? N2 C14 1.2951(10) . ? N2 C13 1.4112(12) . ? C2 C3 1.3869(12) . ? C2 C21 1.5334(14) . ? N3 C37 1.3222(11) . ? N3 C43 1.3939(12) . ? C3 C4 1.4120(15) . ? N4 C37 1.3527(13) . ? N4 C38 1.3854(12) . ? N4 C44 1.4624(12) . ? C4 C5 1.3741(12) . ? C4 C25 1.5314(12) . ? C5 C6 1.4207(12) . ? C6 C7 1.4343(12) . ? C8 C9 1.3943(12) . ? C8 C13 1.4125(11) . ? C9 C10 1.3885(14) . ? C10 C11 1.3958(12) . ? C11 C12 1.3851(14) . ? C12 C13 1.4012(13) . ? C14 C15 1.4357(13) . ? C15 C16 1.4109(11) . ? C15 C20 1.4372(12) . ? C16 C17 1.3757(12) . ? C17 C18 1.4120(13) . ? C17 C29 1.5357(11) . ? C18 C19 1.3941(11) . ? C19 C20 1.4403(11) . ? C19 C33 1.5449(12) . ? C21 C24 1.5386(12) . ? C21 C23 1.5405(11) . ? C21 C22 1.5431(14) . ? C25 C28 1.5289(16) . ? C25 C26 1.5404(12) . ? C25 C27 1.5407(14) . ? C29 C32 1.5329(13) . ? C29 C30 1.5402(17) . ? C29 C31 1.5423(14) . ? C33 C34 1.5348(12) . ? C33 C35 1.5399(15) . ? C33 C36 1.5410(14) . ? C38 C39 1.3963(14) . ? C38 C43 1.4036(13) . ? C39 C40 1.3876(15) . ? C40 C41 1.4100(16) . ? C41 C42 1.3876(15) . ? C42 C43 1.3995(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 96.05(3) . . ? O1 Zn1 N1 88.34(3) . . ? O2 Zn1 N1 150.95(3) . . ? O1 Zn1 N3 102.30(3) . . ? O2 Zn1 N3 104.57(3) . . ? N1 Zn1 N3 102.47(3) . . ? O1 Zn1 N2 158.48(3) . . ? O2 Zn1 N2 88.94(3) . . ? N1 Zn1 N2 77.56(3) . . ? N3 Zn1 N2 96.62(3) . . ? C1 O1 Zn1 131.63(7) . . ? C7 N1 C8 119.44(9) . . ? C7 N1 Zn1 125.15(6) . . ? C8 N1 Zn1 114.14(5) . . ? O1 C1 C6 123.05(8) . . ? O1 C1 C2 119.59(9) . . ? C6 C1 C2 117.36(7) . . ? C20 O2 Zn1 130.01(6) . . ? C14 N2 C13 121.94(8) . . ? C14 N2 Zn1 123.32(7) . . ? C13 N2 Zn1 114.30(5) . . ? C3 C2 C1 118.25(9) . . ? C3 C2 C21 121.91(8) . . ? C1 C2 C21 119.83(7) . . ? C37 N3 C43 105.08(8) . . ? C37 N3 Zn1 124.65(6) . . ? C43 N3 Zn1 130.25(6) . . ? C2 C3 C4 124.79(8) . . ? C37 N4 C38 106.82(7) . . ? C37 N4 C44 126.70(8) . . ? C38 N4 C44 126.38(9) . . ? C5 C4 C3 116.66(8) . . ? C5 C4 C25 122.80(9) . . ? C3 C4 C25 120.53(8) . . ? C4 C5 C6 121.93(9) . . ? C5 C6 C1 120.99(8) . . ? C5 C6 C7 114.94(9) . . ? C1 C6 C7 124.04(8) . . ? N1 C7 C6 126.28(9) . . ? C9 C8 N1 124.12(7) . . ? C9 C8 C13 119.81(8) . . ? N1 C8 C13 116.06(8) . . ? C10 C9 C8 120.15(8) . . ? C9 C10 C11 120.09(9) . . ? C12 C11 C10 120.15(9) . . ? C11 C12 C13 120.42(8) . . ? C12 C13 N2 126.08(7) . . ? C12 C13 C8 119.02(8) . . ? N2 C13 C8 114.87(7) . . ? N2 C14 C15 126.12(8) . . ? C16 C15 C14 114.47(8) . . ? C16 C15 C20 120.72(8) . . ? C14 C15 C20 124.44(7) . . ? C17 C16 C15 122.63(8) . . ? C16 C17 C18 116.17(7) . . ? C16 C17 C29 119.51(8) . . ? C18 C17 C29 124.28(8) . . ? C19 C18 C17 124.59(8) . . ? C18 C19 C20 118.64(8) . . ? C18 C19 C33 121.17(7) . . ? C20 C19 C33 120.19(7) . . ? O2 C20 C15 122.99(7) . . ? O2 C20 C19 120.24(8) . . ? C15 C20 C19 116.77(7) . . ? C2 C21 C24 111.93(7) . . ? C2 C21 C23 109.87(8) . . ? C24 C21 C23 107.75(7) . . ? C2 C21 C22 110.60(7) . . ? C24 C21 C22 107.52(9) . . ? C23 C21 C22 109.07(7) . . ? C28 C25 C4 112.36(7) . . ? C28 C25 C26 108.40(10) . . ? C4 C25 C26 109.04(7) . . ? C28 C25 C27 107.93(8) . . ? C4 C25 C27 109.75(9) . . ? C26 C25 C27 109.30(8) . . ? C32 C29 C17 112.25(7) . . ? C32 C29 C30 108.59(8) . . ? C17 C29 C30 109.38(8) . . ? C32 C29 C31 108.25(9) . . ? C17 C29 C31 109.36(7) . . ? C30 C29 C31 108.94(9) . . ? C34 C33 C35 107.16(9) . . ? C34 C33 C36 106.88(7) . . ? C35 C33 C36 108.92(8) . . ? C34 C33 C19 112.03(7) . . ? C35 C33 C19 111.26(7) . . ? C36 C33 C19 110.41(9) . . ? N3 C37 N4 113.30(8) . . ? N4 C38 C39 131.52(9) . . ? N4 C38 C43 105.65(8) . . ? C39 C38 C43 122.81(9) . . ? C40 C39 C38 116.27(9) . . ? C39 C40 C41 121.45(10) . . ? C42 C41 C40 121.94(9) . . ? C41 C42 C43 117.11(9) . . ? N3 C43 C42 130.48(8) . . ? N3 C43 C38 109.14(7) . . ? C42 C43 C38 120.38(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 O1 C1 138.84(7) . . . . ? N1 Zn1 O1 C1 -12.38(7) . . . . ? N3 Zn1 O1 C1 -114.77(7) . . . . ? N2 Zn1 O1 C1 36.25(11) . . . . ? O1 Zn1 N1 C7 12.31(7) . . . . ? O2 Zn1 N1 C7 -87.19(9) . . . . ? N3 Zn1 N1 C7 114.54(7) . . . . ? N2 Zn1 N1 C7 -151.32(8) . . . . ? O1 Zn1 N1 C8 179.31(6) . . . . ? O2 Zn1 N1 C8 79.81(7) . . . . ? N3 Zn1 N1 C8 -78.46(6) . . . . ? N2 Zn1 N1 C8 15.68(5) . . . . ? Zn1 O1 C1 C6 8.85(12) . . . . ? Zn1 O1 C1 C2 -171.72(6) . . . . ? O1 Zn1 O2 C20 -174.00(8) . . . . ? N1 Zn1 O2 C20 -76.49(10) . . . . ? N3 Zn1 O2 C20 81.58(9) . . . . ? N2 Zn1 O2 C20 -14.98(9) . . . . ? O1 Zn1 N2 C14 123.81(8) . . . . ? O2 Zn1 N2 C14 19.91(7) . . . . ? N1 Zn1 N2 C14 174.00(7) . . . . ? N3 Zn1 N2 C14 -84.64(7) . . . . ? O1 Zn1 N2 C13 -63.68(9) . . . . ? O2 Zn1 N2 C13 -167.59(6) . . . . ? N1 Zn1 N2 C13 -13.49(6) . . . . ? N3 Zn1 N2 C13 87.87(6) . . . . ? O1 C1 C2 C3 178.73(7) . . . . ? C6 C1 C2 C3 -1.81(11) . . . . ? O1 C1 C2 C21 -0.39(11) . . . . ? C6 C1 C2 C21 179.07(7) . . . . ? O1 Zn1 N3 C37 -156.86(8) . . . . ? O2 Zn1 N3 C37 -57.18(9) . . . . ? N1 Zn1 N3 C37 112.12(8) . . . . ? N2 Zn1 N3 C37 33.45(9) . . . . ? O1 Zn1 N3 C43 21.15(9) . . . . ? O2 Zn1 N3 C43 120.83(8) . . . . ? N1 Zn1 N3 C43 -69.87(9) . . . . ? N2 Zn1 N3 C43 -148.55(9) . . . . ? C1 C2 C3 C4 1.09(13) . . . . ? C21 C2 C3 C4 -179.81(8) . . . . ? C2 C3 C4 C5 -0.60(13) . . . . ? C2 C3 C4 C25 -178.97(8) . . . . ? C3 C4 C5 C6 0.89(12) . . . . ? C25 C4 C5 C6 179.22(8) . . . . ? C4 C5 C6 C1 -1.75(13) . . . . ? C4 C5 C6 C7 -179.94(8) . . . . ? O1 C1 C6 C5 -178.40(8) . . . . ? C2 C1 C6 C5 2.16(12) . . . . ? O1 C1 C6 C7 -0.38(13) . . . . ? C2 C1 C6 C7 -179.82(8) . . . . ? C8 N1 C7 C6 -176.22(8) . . . . ? Zn1 N1 C7 C6 -9.85(12) . . . . ? C5 C6 C7 N1 179.74(8) . . . . ? C1 C6 C7 N1 1.61(14) . . . . ? C7 N1 C8 C9 -28.68(12) . . . . ? Zn1 N1 C8 C9 163.51(7) . . . . ? C7 N1 C8 C13 151.85(8) . . . . ? Zn1 N1 C8 C13 -15.95(9) . . . . ? N1 C8 C9 C10 175.32(9) . . . . ? C13 C8 C9 C10 -5.23(14) . . . . ? C8 C9 C10 C11 0.07(15) . . . . ? C9 C10 C11 C12 3.82(15) . . . . ? C10 C11 C12 C13 -2.49(14) . . . . ? C11 C12 C13 N2 179.24(8) . . . . ? C11 C12 C13 C8 -2.63(13) . . . . ? C14 N2 C13 C12 0.04(13) . . . . ? Zn1 N2 C13 C12 -172.58(7) . . . . ? C14 N2 C13 C8 -178.15(8) . . . . ? Zn1 N2 C13 C8 9.23(9) . . . . ? C9 C8 C13 C12 6.48(13) . . . . ? N1 C8 C13 C12 -174.03(8) . . . . ? C9 C8 C13 N2 -175.19(8) . . . . ? N1 C8 C13 N2 4.30(11) . . . . ? C13 N2 C14 C15 174.92(8) . . . . ? Zn1 N2 C14 C15 -13.13(12) . . . . ? N2 C14 C15 C16 179.94(9) . . . . ? N2 C14 C15 C20 -7.02(15) . . . . ? C14 C15 C16 C17 171.40(9) . . . . ? C20 C15 C16 C17 -1.92(15) . . . . ? C15 C16 C17 C18 -2.91(15) . . . . ? C15 C16 C17 C29 179.09(9) . . . . ? C16 C17 C18 C19 2.52(15) . . . . ? C29 C17 C18 C19 -179.60(9) . . . . ? C17 C18 C19 C20 2.73(15) . . . . ? C17 C18 C19 C33 -176.74(9) . . . . ? Zn1 O2 C20 C15 1.96(14) . . . . ? Zn1 O2 C20 C19 -178.66(7) . . . . ? C16 C15 C20 O2 -173.55(9) . . . . ? C14 C15 C20 O2 13.83(15) . . . . ? C16 C15 C20 C19 7.05(13) . . . . ? C14 C15 C20 C19 -165.57(9) . . . . ? C18 C19 C20 O2 173.27(9) . . . . ? C33 C19 C20 O2 -7.26(14) . . . . ? C18 C19 C20 C15 -7.32(13) . . . . ? C33 C19 C20 C15 172.16(9) . . . . ? C3 C2 C21 C24 0.75(11) . . . . ? C1 C2 C21 C24 179.84(7) . . . . ? C3 C2 C21 C23 -118.91(8) . . . . ? C1 C2 C21 C23 60.18(9) . . . . ? C3 C2 C21 C22 120.62(8) . . . . ? C1 C2 C21 C22 -60.29(10) . . . . ? C5 C4 C25 C28 9.07(13) . . . . ? C3 C4 C25 C28 -172.66(9) . . . . ? C5 C4 C25 C26 -111.13(10) . . . . ? C3 C4 C25 C26 67.13(12) . . . . ? C5 C4 C25 C27 129.16(9) . . . . ? C3 C4 C25 C27 -52.57(10) . . . . ? C16 C17 C29 C32 176.46(9) . . . . ? C18 C17 C29 C32 -1.36(14) . . . . ? C16 C17 C29 C30 55.85(11) . . . . ? C18 C17 C29 C30 -121.97(10) . . . . ? C16 C17 C29 C31 -63.38(13) . . . . ? C18 C17 C29 C31 118.80(11) . . . . ? C18 C19 C33 C34 2.92(14) . . . . ? C20 C19 C33 C34 -176.54(9) . . . . ? C18 C19 C33 C35 -117.01(10) . . . . ? C20 C19 C33 C35 63.53(12) . . . . ? C18 C19 C33 C36 121.92(9) . . . . ? C20 C19 C33 C36 -57.54(11) . . . . ? C43 N3 C37 N4 -0.28(12) . . . . ? Zn1 N3 C37 N4 178.15(7) . . . . ? C38 N4 C37 N3 -0.32(12) . . . . ? C44 N4 C37 N3 176.36(9) . . . . ? C37 N4 C38 C39 -177.61(12) . . . . ? C44 N4 C38 C39 5.70(18) . . . . ? C37 N4 C38 C43 0.77(11) . . . . ? C44 N4 C38 C43 -175.92(10) . . . . ? N4 C38 C39 C40 179.21(11) . . . . ? C43 C38 C39 C40 1.06(17) . . . . ? C38 C39 C40 C41 0.43(18) . . . . ? C39 C40 C41 C42 -1.1(2) . . . . ? C40 C41 C42 C43 0.24(18) . . . . ? C37 N3 C43 C42 -179.76(11) . . . . ? Zn1 N3 C43 C42 1.94(16) . . . . ? C37 N3 C43 C38 0.77(11) . . . . ? Zn1 N3 C43 C38 -177.54(7) . . . . ? C41 C42 C43 N3 -178.21(11) . . . . ? C41 C42 C43 C38 1.22(15) . . . . ? N4 C38 C43 N3 -0.96(11) . . . . ? C39 C38 C43 N3 177.60(10) . . . . ? N4 C38 C43 C42 179.51(9) . . . . ? C39 C38 C43 C42 -1.94(16) . . . . ? _diffrn_measured_fraction_theta_max 0.693 _diffrn_reflns_theta_full 39.97 _diffrn_measured_fraction_theta_full 0.693 _refine_diff_density_max 0.677 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.068 # Attachment 'AWK09b_0m.cif' data_awk09b_0m _database_code_depnum_ccdc_archive 'CCDC 658374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H105 N7 O4' _chemical_formula_weight 1204.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9668(6) _cell_length_b 11.7206(5) _cell_length_c 33.5724(16) _cell_angle_alpha 81.394(2) _cell_angle_beta 82.282(2) _cell_angle_gamma 69.164(2) _cell_volume 3610.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5446 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 35.03 _exptl_crystal_description Block _exptl_crystal_colour translucent _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.812309 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58825 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 35.18 _reflns_number_total 29202 _reflns_number_gt 19213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+2.4277P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 29202 _refine_ls_number_parameters 833 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.2059 _refine_ls_wR_factor_gt 0.1862 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 1.00288(13) 0.12824(13) 0.12980(4) 0.0223(2) Uani 1 1 d . . . H1A H 0.9628 0.1536 0.1520 0.033 Uiso 1 1 calc R . . C1A C 1.14355(16) 0.11720(14) 0.12686(5) 0.0155(3) Uani 1 1 d . . . N1A N 0.98085(14) 0.18653(12) 0.20260(4) 0.0164(2) Uani 1 1 d . . . O2A O 0.74296(12) 0.47999(12) 0.13225(4) 0.0201(2) Uani 1 1 d . . . H2A H 0.7666 0.4390 0.1545 0.030 Uiso 1 1 calc R . . C2A C 1.23118(16) 0.08628(14) 0.09038(5) 0.0151(3) Uani 1 1 d . . . N2A N 0.71330(14) 0.36759(12) 0.20360(4) 0.0152(2) Uani 1 1 d . . . C3A C 1.37397(16) 0.07946(14) 0.08896(5) 0.0149(3) Uani 1 1 d . . . H3A H 1.4331 0.0602 0.0645 0.018 Uiso 1 1 calc R . . C4A C 1.43669(16) 0.09905(13) 0.12117(5) 0.0145(3) Uani 1 1 d . . . C5A C 1.34896(16) 0.12646(14) 0.15667(5) 0.0152(3) Uani 1 1 d . . . H5A H 1.3879 0.1394 0.1792 0.018 Uiso 1 1 calc R . . C6A C 1.20322(16) 0.13556(14) 0.15996(4) 0.0144(3) Uani 1 1 d . . . C7A C 1.11696(16) 0.16830(14) 0.19784(4) 0.0157(3) Uani 1 1 d . . . H7A H 1.1627 0.1765 0.2198 0.019 Uiso 1 1 calc R . . C8A C 1.17057(18) 0.06186(16) 0.05415(5) 0.0186(3) Uani 1 1 d . . . C9A C 1.1169(2) -0.04733(19) 0.06674(6) 0.0283(4) Uani 1 1 d . . . H9A1 H 1.0423 -0.0284 0.0894 0.042 Uiso 1 1 calc R . . H9A2 H 1.1976 -0.1207 0.0751 0.042 Uiso 1 1 calc R . . H9A3 H 1.0766 -0.0625 0.0438 0.042 Uiso 1 1 calc R . . C10A C 1.0476(2) 0.17704(19) 0.03923(6) 0.0287(4) Uani 1 1 d . . . H10A H 0.9718 0.2006 0.0613 0.043 Uiso 1 1 calc R . . H10B H 1.0078 0.1595 0.0166 0.043 Uiso 1 1 calc R . . H10C H 1.0848 0.2445 0.0302 0.043 Uiso 1 1 calc R . . C11A C 1.28604(19) 0.02726(17) 0.01853(5) 0.0227(3) Uani 1 1 d . . . H11A H 1.2439 0.0103 -0.0037 0.034 Uiso 1 1 calc R . . H11B H 1.3660 -0.0461 0.0273 0.034 Uiso 1 1 calc R . . H11C H 1.3218 0.0955 0.0093 0.034 Uiso 1 1 calc R . . C12A C 1.59409(16) 0.09300(14) 0.11582(5) 0.0160(3) Uani 1 1 d . . . C13A C 1.60898(19) 0.19977(17) 0.08477(6) 0.0250(3) Uani 1 1 d . . . H13A H 1.5818 0.1918 0.0586 0.038 Uiso 1 1 calc R . . H13B H 1.7091 0.1974 0.0818 0.038 Uiso 1 1 calc R . . H13C H 1.5455 0.2780 0.0942 0.038 Uiso 1 1 calc R . . C14A C 1.69097(17) -0.02895(15) 0.10007(5) 0.0195(3) Uani 1 1 d . . . H14A H 1.6797 -0.0976 0.1191 0.029 Uiso 1 1 calc R . . H14B H 1.7918 -0.0333 0.0974 0.029 Uiso 1 1 calc R . . H14C H 1.6632 -0.0337 0.0736 0.029 Uiso 1 1 calc R . . C15A C 1.64656(18) 0.10195(16) 0.15566(5) 0.0213(3) Uani 1 1 d . . . H15A H 1.5902 0.1817 0.1652 0.032 Uiso 1 1 calc R . . H15B H 1.7486 0.0938 0.1514 0.032 Uiso 1 1 calc R . . H15C H 1.6344 0.0361 0.1759 0.032 Uiso 1 1 calc R . . C16A C 0.90409(16) 0.21598(14) 0.24068(4) 0.0156(3) Uani 1 1 d . . . C17A C 0.95913(17) 0.15456(15) 0.27718(5) 0.0186(3) Uani 1 1 d . . . H17A H 1.0520 0.0929 0.2770 0.022 Uiso 1 1 calc R . . C18A C 0.87860(19) 0.18321(16) 0.31385(5) 0.0220(3) Uani 1 1 d . . . H18A H 0.9167 0.1412 0.3385 0.026 Uiso 1 1 calc R . . C19A C 0.74237(19) 0.27324(16) 0.31444(5) 0.0214(3) Uani 1 1 d . . . H19A H 0.6880 0.2931 0.3395 0.026 Uiso 1 1 calc R . . C20A C 0.68543(18) 0.33453(15) 0.27815(5) 0.0183(3) Uani 1 1 d . . . H20A H 0.5925 0.3960 0.2786 0.022 Uiso 1 1 calc R . . C21A C 0.76494(16) 0.30565(14) 0.24112(4) 0.0147(3) Uani 1 1 d . . . C22A C 0.58040(16) 0.39037(14) 0.19790(4) 0.0148(3) Uani 1 1 d . . . H22A H 0.5191 0.3670 0.2192 0.018 Uiso 1 1 calc R . . C23A C 0.52170(16) 0.45074(14) 0.15987(4) 0.0143(3) Uani 1 1 d . . . C24A C 0.37981(16) 0.46150(14) 0.15489(5) 0.0157(3) Uani 1 1 d . . . H24A H 0.3244 0.4333 0.1768 0.019 Uiso 1 1 calc R . . C25A C 0.31912(16) 0.51215(14) 0.11889(5) 0.0147(3) Uani 1 1 d . . . C26A C 0.40502(16) 0.55432(14) 0.08749(5) 0.0148(3) Uani 1 1 d . . . H26A H 0.3641 0.5899 0.0626 0.018 Uiso 1 1 calc R . . C27A C 0.54595(16) 0.54720(13) 0.09054(4) 0.0138(2) Uani 1 1 d . . . C28A C 0.60537(15) 0.49253(14) 0.12760(5) 0.0144(3) Uani 1 1 d . . . C29A C 0.16786(16) 0.52016(15) 0.11138(5) 0.0184(3) Uani 1 1 d . . . C30A C 0.1806(2) 0.43162(18) 0.08063(6) 0.0270(4) Uani 1 1 d . . . H30A H 0.2298 0.4550 0.0551 0.040 Uiso 1 1 calc R . . H30B H 0.0841 0.4355 0.0759 0.040 Uiso 1 1 calc R . . H30C H 0.2361 0.3477 0.0912 0.040 Uiso 1 1 calc R . . C31A C 0.08114(18) 0.65145(17) 0.09449(6) 0.0259(4) Uani 1 1 d . . . H31A H 0.0784 0.7091 0.1132 0.039 Uiso 1 1 calc R . . H31B H -0.0174 0.6566 0.0914 0.039 Uiso 1 1 calc R . . H31C H 0.1270 0.6723 0.0681 0.039 Uiso 1 1 calc R . . C32A C 0.08579(18) 0.48438(17) 0.15042(6) 0.0240(3) Uani 1 1 d . . . H32A H 0.1386 0.3998 0.1611 0.036 Uiso 1 1 calc R . . H32B H -0.0104 0.4904 0.1446 0.036 Uiso 1 1 calc R . . H32C H 0.0768 0.5400 0.1705 0.036 Uiso 1 1 calc R . . C33A C 0.63355(16) 0.59585(14) 0.05529(5) 0.0157(3) Uani 1 1 d . . . C34A C 0.76887(19) 0.49009(17) 0.04177(5) 0.0249(3) Uani 1 1 d . . . H34A H 0.8263 0.4516 0.0648 0.037 Uiso 1 1 calc R . . H34B H 0.8266 0.5226 0.0202 0.037 Uiso 1 1 calc R . . H34C H 0.7398 0.4289 0.0317 0.037 Uiso 1 1 calc R . . C35A C 0.6759(2) 0.69685(18) 0.06896(5) 0.0248(3) Uani 1 1 d . . . H35A H 0.5887 0.7660 0.0755 0.037 Uiso 1 1 calc R . . H35B H 0.7364 0.7250 0.0471 0.037 Uiso 1 1 calc R . . H35C H 0.7295 0.6640 0.0930 0.037 Uiso 1 1 calc R . . C36A C 0.54741(18) 0.65323(15) 0.01851(5) 0.0195(3) Uani 1 1 d . . . H36A H 0.5207 0.5907 0.0084 0.029 Uiso 1 1 calc R . . H36B H 0.6064 0.6853 -0.0028 0.029 Uiso 1 1 calc R . . H36C H 0.4600 0.7204 0.0263 0.029 Uiso 1 1 calc R . . C1B C 0.33402(16) 0.48400(14) 0.62318(5) 0.0159(3) Uani 1 1 d . . . O1B O 0.20442(13) 0.46906(12) 0.63008(4) 0.0207(2) Uani 1 1 d . . . H1B H 0.1997 0.4276 0.6526 0.031 Uiso 1 1 calc R . . N1B N 0.27895(15) 0.35846(13) 0.69962(4) 0.0181(2) Uani 1 1 d . . . C2B C 0.36827(16) 0.54765(14) 0.58614(5) 0.0157(3) Uani 1 1 d . . . O2B O 0.23661(13) 0.14072(12) 0.63034(4) 0.0197(2) Uani 1 1 d . . . H2B H 0.2326 0.1660 0.6527 0.030 Uiso 1 1 calc R . . N2B N 0.13511(15) 0.20152(13) 0.70171(4) 0.0173(2) Uani 1 1 d . . . C3B C 0.50316(17) 0.56127(15) 0.58055(5) 0.0176(3) Uani 1 1 d . . . H3B H 0.5273 0.6034 0.5558 0.021 Uiso 1 1 calc R . . C4B C 0.60559(17) 0.51678(15) 0.60915(5) 0.0188(3) Uani 1 1 d . . . C5B C 0.56875(17) 0.45549(15) 0.64528(5) 0.0186(3) Uani 1 1 d . . . H5B H 0.6354 0.4245 0.6653 0.022 Uiso 1 1 calc R . . C6B C 0.43437(16) 0.43860(14) 0.65267(5) 0.0161(3) Uani 1 1 d . . . C7B C 0.40044(18) 0.37657(15) 0.69140(5) 0.0181(3) Uani 1 1 d . . . H7B H 0.4689 0.3489 0.7110 0.022 Uiso 1 1 calc R . . C8B C 0.25939(17) 0.60199(15) 0.55422(5) 0.0173(3) Uani 1 1 d . . . C9B C 0.12352(18) 0.69928(16) 0.57216(6) 0.0230(3) Uani 1 1 d . . . H9B1 H 0.0793 0.6604 0.5955 0.034 Uiso 1 1 calc R . . H9B2 H 0.0546 0.7353 0.5516 0.034 Uiso 1 1 calc R . . H9B3 H 0.1505 0.7639 0.5807 0.034 Uiso 1 1 calc R . . C10B C 0.2195(2) 0.50007(17) 0.54051(5) 0.0240(3) Uani 1 1 d . . . H10D H 0.3063 0.4398 0.5287 0.036 Uiso 1 1 calc R . . H10E H 0.1496 0.5358 0.5202 0.036 Uiso 1 1 calc R . . H10F H 0.1771 0.4595 0.5638 0.036 Uiso 1 1 calc R . . C11B C 0.31940(19) 0.66553(16) 0.51626(5) 0.0216(3) Uani 1 1 d . . . H11D H 0.3437 0.7331 0.5237 0.032 Uiso 1 1 calc R . . H11E H 0.2466 0.6980 0.4967 0.032 Uiso 1 1 calc R . . H11F H 0.4061 0.6060 0.5042 0.032 Uiso 1 1 calc R . . C12B C 0.7548(2) 0.53006(19) 0.59956(6) 0.0276(4) Uani 1 1 d . . . C13B C 0.8571(2) 0.4143(2) 0.57967(8) 0.0406(5) Uani 1 1 d . . . H13D H 0.9541 0.4192 0.5740 0.061 Uiso 1 1 calc R . . H13E H 0.8208 0.4107 0.5543 0.061 Uiso 1 1 calc R . . H13F H 0.8607 0.3404 0.5981 0.061 Uiso 1 1 calc R . . C14B C 0.7511(2) 0.64087(19) 0.56841(7) 0.0324(4) Uani 1 1 d . . . H14D H 0.6763 0.7148 0.5776 0.049 Uiso 1 1 calc R . . H14E H 0.7298 0.6266 0.5423 0.049 Uiso 1 1 calc R . . H14F H 0.8450 0.6521 0.5654 0.049 Uiso 1 1 calc R . . C15B C 0.8172(3) 0.5370(4) 0.63702(8) 0.0562(8) Uani 1 1 d . . . H15D H 0.7557 0.6107 0.6495 0.084 Uiso 1 1 calc R . . H15E H 0.9141 0.5410 0.6299 0.084 Uiso 1 1 calc R . . H15F H 0.8224 0.4640 0.6561 0.084 Uiso 1 1 calc R . . C16B C 0.24050(17) 0.30515(14) 0.73786(5) 0.0173(3) Uani 1 1 d . . . C17B C 0.27095(19) 0.33188(16) 0.77407(5) 0.0211(3) Uani 1 1 d . . . H17B H 0.3268 0.3831 0.7735 0.025 Uiso 1 1 calc R . . C18B C 0.2198(2) 0.28368(17) 0.81099(5) 0.0238(3) Uani 1 1 d . . . H18B H 0.2411 0.3021 0.8355 0.029 Uiso 1 1 calc R . . C19B C 0.13830(19) 0.20921(16) 0.81212(5) 0.0227(3) Uani 1 1 d . . . H19B H 0.1038 0.1765 0.8374 0.027 Uiso 1 1 calc R . . C20B C 0.10686(18) 0.18233(16) 0.77632(5) 0.0207(3) Uani 1 1 d . . . H20B H 0.0517 0.1304 0.7772 0.025 Uiso 1 1 calc R . . C21B C 0.15587(17) 0.23117(14) 0.73903(4) 0.0166(3) Uani 1 1 d . . . C22B C 0.01950(17) 0.18168(14) 0.69654(5) 0.0169(3) Uani 1 1 d . . . H22B H -0.0560 0.1931 0.7177 0.020 Uiso 1 1 calc R . . C23B C 0.00229(16) 0.14251(14) 0.65932(5) 0.0156(3) Uani 1 1 d . . . C24B C -0.12670(16) 0.12314(14) 0.65599(5) 0.0163(3) Uani 1 1 d . . . H24B H -0.1997 0.1368 0.6779 0.020 Uiso 1 1 calc R . . C25B C -0.14891(16) 0.08449(14) 0.62134(5) 0.0159(3) Uani 1 1 d . . . C26B C -0.03769(16) 0.06645(14) 0.58958(5) 0.0162(3) Uani 1 1 d . . . H26B H -0.0527 0.0404 0.5656 0.019 Uiso 1 1 calc R . . C27B C 0.09262(16) 0.08424(14) 0.59099(4) 0.0147(3) Uani 1 1 d . . . C28B C 0.11226(16) 0.12278(14) 0.62701(5) 0.0153(3) Uani 1 1 d . . . C29B C -0.28767(17) 0.06265(15) 0.61598(5) 0.0184(3) Uani 1 1 d . . . C30B C -0.39129(19) 0.07911(19) 0.65456(6) 0.0272(4) Uani 1 1 d . . . H30D H -0.3441 0.0207 0.6768 0.041 Uiso 1 1 calc R . . H30E H -0.4784 0.0640 0.6500 0.041 Uiso 1 1 calc R . . H30F H -0.4175 0.1631 0.6615 0.041 Uiso 1 1 calc R . . C31B C -0.2516(2) -0.06868(17) 0.60577(7) 0.0280(4) Uani 1 1 d . . . H31D H -0.1859 -0.0814 0.5811 0.042 Uiso 1 1 calc R . . H31E H -0.3404 -0.0815 0.6016 0.042 Uiso 1 1 calc R . . H31F H -0.2054 -0.1272 0.6281 0.042 Uiso 1 1 calc R . . C32B C -0.3647(2) 0.15541(19) 0.58150(6) 0.0276(4) Uani 1 1 d . . . H32D H -0.3864 0.2392 0.5881 0.041 Uiso 1 1 calc R . . H32E H -0.4545 0.1428 0.5783 0.041 Uiso 1 1 calc R . . H32F H -0.3019 0.1432 0.5562 0.041 Uiso 1 1 calc R . . C33B C 0.20940(17) 0.06397(15) 0.55531(5) 0.0172(3) Uani 1 1 d . . . C34B C 0.1624(2) 0.02700(17) 0.51908(5) 0.0230(3) Uani 1 1 d . . . H34D H 0.2400 0.0143 0.4971 0.034 Uiso 1 1 calc R . . H34E H 0.0757 0.0923 0.5098 0.034 Uiso 1 1 calc R . . H34F H 0.1415 -0.0493 0.5271 0.034 Uiso 1 1 calc R . . C35B C 0.2415(2) 0.18332(17) 0.54059(5) 0.0241(3) Uani 1 1 d . . . H35D H 0.3167 0.1689 0.5180 0.036 Uiso 1 1 calc R . . H35E H 0.2744 0.2092 0.5628 0.036 Uiso 1 1 calc R . . H35F H 0.1537 0.2478 0.5316 0.036 Uiso 1 1 calc R . . C36B C 0.34791(18) -0.03954(17) 0.56835(6) 0.0228(3) Uani 1 1 d . . . H36D H 0.3262 -0.1148 0.5780 0.034 Uiso 1 1 calc R . . H36E H 0.3846 -0.0151 0.5901 0.034 Uiso 1 1 calc R . . H36F H 0.4208 -0.0545 0.5452 0.034 Uiso 1 1 calc R . . N1S N 0.3698(2) 0.21674(19) 0.25576(7) 0.0406(4) Uani 1 1 d . . . C1S C 0.4763(2) 0.14676(18) 0.26545(6) 0.0292(4) Uani 1 1 d . . . C2S C 0.6134(2) 0.0570(2) 0.27694(8) 0.0419(6) Uani 1 1 d . . . H2S1 H 0.6132 -0.0260 0.2757 0.063 Uiso 1 1 calc R . . H2S2 H 0.6273 0.0656 0.3045 0.063 Uiso 1 1 calc R . . H2S3 H 0.6919 0.0710 0.2583 0.063 Uiso 1 1 calc R . . C1T C 0.6763(3) 0.1610(2) 0.78762(8) 0.0479(6) Uani 1 1 d . . . N1T N 0.6992(4) 0.1218(3) 0.75723(8) 0.0782(10) Uani 1 1 d . . . C2T C 0.6480(4) 0.2077(3) 0.82673(9) 0.0597(8) Uani 1 1 d . . . H2T1 H 0.6831 0.1394 0.8478 0.090 Uiso 1 1 calc R . . H2T2 H 0.5441 0.2488 0.8324 0.090 Uiso 1 1 calc R . . H2T3 H 0.6977 0.2665 0.8264 0.090 Uiso 1 1 calc R . . C1R C 0.1793(4) 0.5158(3) 0.25963(8) 0.0559(8) Uani 1 1 d . . . N1R N 0.2634(4) 0.5654(3) 0.25282(8) 0.0747(9) Uani 1 1 d . . . C2R C 0.0751(3) 0.4524(3) 0.26859(9) 0.0584(8) Uani 1 1 d . . . H2R1 H 0.1261 0.3635 0.2714 0.088 Uiso 1 1 calc R . . H2R2 H 0.0123 0.4746 0.2465 0.088 Uiso 1 1 calc R . . H2R3 H 0.0167 0.4765 0.2939 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.0148(5) 0.0378(7) 0.0192(5) -0.0099(5) 0.0027(4) -0.0139(5) C1A 0.0124(6) 0.0183(7) 0.0174(6) -0.0029(5) -0.0002(5) -0.0072(5) N1A 0.0152(6) 0.0189(6) 0.0143(5) -0.0019(4) 0.0012(4) -0.0058(4) O2A 0.0141(5) 0.0303(6) 0.0185(5) 0.0048(4) -0.0050(4) -0.0125(4) C2A 0.0147(6) 0.0159(6) 0.0160(6) -0.0019(5) -0.0004(5) -0.0069(5) N2A 0.0159(6) 0.0163(6) 0.0139(5) -0.0019(4) -0.0022(4) -0.0058(4) C3A 0.0143(6) 0.0146(6) 0.0162(6) -0.0026(5) 0.0009(5) -0.0059(5) C4A 0.0128(6) 0.0138(6) 0.0175(6) -0.0017(5) -0.0004(5) -0.0059(5) C5A 0.0138(6) 0.0169(6) 0.0160(6) -0.0024(5) -0.0015(5) -0.0063(5) C6A 0.0124(6) 0.0159(6) 0.0149(6) -0.0017(5) 0.0008(5) -0.0056(5) C7A 0.0144(6) 0.0177(6) 0.0147(6) -0.0018(5) -0.0001(5) -0.0056(5) C8A 0.0196(7) 0.0227(7) 0.0162(6) -0.0042(5) -0.0018(5) -0.0096(6) C9A 0.0328(10) 0.0358(10) 0.0270(8) -0.0093(7) 0.0021(7) -0.0242(8) C10A 0.0236(8) 0.0365(10) 0.0243(8) -0.0062(7) -0.0077(7) -0.0050(7) C11A 0.0238(8) 0.0294(9) 0.0174(7) -0.0058(6) 0.0011(6) -0.0119(6) C12A 0.0119(6) 0.0166(6) 0.0201(7) -0.0022(5) 0.0006(5) -0.0063(5) C13A 0.0194(8) 0.0232(8) 0.0336(9) 0.0030(7) -0.0003(6) -0.0118(6) C14A 0.0154(7) 0.0221(7) 0.0205(7) -0.0052(6) -0.0004(5) -0.0050(5) C15A 0.0159(7) 0.0239(8) 0.0273(8) -0.0093(6) -0.0016(6) -0.0085(6) C16A 0.0152(6) 0.0181(7) 0.0131(6) -0.0020(5) 0.0003(5) -0.0058(5) C17A 0.0178(7) 0.0193(7) 0.0158(6) 0.0002(5) -0.0020(5) -0.0034(5) C18A 0.0256(8) 0.0233(8) 0.0141(6) 0.0001(5) -0.0024(6) -0.0055(6) C19A 0.0255(8) 0.0216(7) 0.0141(6) -0.0040(5) 0.0014(5) -0.0047(6) C20A 0.0195(7) 0.0175(7) 0.0153(6) -0.0033(5) 0.0003(5) -0.0031(5) C21A 0.0152(6) 0.0152(6) 0.0133(6) -0.0014(5) -0.0012(5) -0.0048(5) C22A 0.0149(6) 0.0145(6) 0.0158(6) -0.0027(5) -0.0001(5) -0.0059(5) C23A 0.0133(6) 0.0153(6) 0.0146(6) -0.0018(5) -0.0016(5) -0.0052(5) C24A 0.0120(6) 0.0160(6) 0.0198(6) -0.0029(5) 0.0000(5) -0.0057(5) C25A 0.0118(6) 0.0146(6) 0.0195(6) -0.0036(5) -0.0016(5) -0.0057(5) C26A 0.0137(6) 0.0150(6) 0.0171(6) -0.0013(5) -0.0036(5) -0.0058(5) C27A 0.0136(6) 0.0146(6) 0.0146(6) -0.0008(5) -0.0024(5) -0.0066(5) C28A 0.0119(6) 0.0156(6) 0.0178(6) -0.0017(5) -0.0028(5) -0.0067(5) C29A 0.0122(6) 0.0179(7) 0.0263(7) -0.0015(6) -0.0024(5) -0.0065(5) C30A 0.0215(8) 0.0305(9) 0.0356(9) -0.0096(7) -0.0061(7) -0.0135(7) C31A 0.0141(7) 0.0236(8) 0.0363(9) 0.0033(7) -0.0039(6) -0.0042(6) C32A 0.0138(7) 0.0254(8) 0.0334(9) -0.0009(7) 0.0005(6) -0.0092(6) C33A 0.0155(6) 0.0182(7) 0.0161(6) 0.0003(5) -0.0026(5) -0.0093(5) C34A 0.0174(7) 0.0301(9) 0.0221(7) 0.0007(6) 0.0009(6) -0.0045(6) C35A 0.0308(9) 0.0294(9) 0.0224(8) 0.0031(6) -0.0061(6) -0.0215(7) C36A 0.0227(8) 0.0201(7) 0.0170(6) 0.0010(5) -0.0041(5) -0.0092(6) C1B 0.0132(6) 0.0166(6) 0.0193(6) -0.0028(5) -0.0010(5) -0.0067(5) O1B 0.0162(5) 0.0280(6) 0.0204(5) 0.0032(4) -0.0026(4) -0.0126(4) N1B 0.0208(6) 0.0185(6) 0.0164(6) -0.0030(5) -0.0008(5) -0.0081(5) C2B 0.0139(6) 0.0163(6) 0.0185(6) -0.0021(5) -0.0019(5) -0.0067(5) O2B 0.0165(5) 0.0294(6) 0.0191(5) -0.0069(4) -0.0002(4) -0.0137(4) N2B 0.0189(6) 0.0202(6) 0.0144(5) -0.0023(5) -0.0023(4) -0.0081(5) C3B 0.0155(6) 0.0196(7) 0.0202(7) -0.0029(5) -0.0007(5) -0.0091(5) C4B 0.0151(7) 0.0189(7) 0.0250(7) -0.0023(6) -0.0035(5) -0.0082(5) C5B 0.0166(7) 0.0183(7) 0.0232(7) -0.0023(5) -0.0056(5) -0.0075(5) C6B 0.0153(6) 0.0159(6) 0.0185(6) -0.0032(5) -0.0018(5) -0.0063(5) C7B 0.0202(7) 0.0168(7) 0.0183(6) -0.0027(5) -0.0047(5) -0.0062(5) C8B 0.0155(7) 0.0187(7) 0.0196(7) -0.0009(5) -0.0029(5) -0.0082(5) C9B 0.0153(7) 0.0242(8) 0.0275(8) 0.0013(6) -0.0028(6) -0.0056(6) C10B 0.0270(8) 0.0291(9) 0.0221(7) -0.0015(6) -0.0054(6) -0.0164(7) C11B 0.0231(8) 0.0236(8) 0.0202(7) 0.0014(6) -0.0030(6) -0.0117(6) C12B 0.0194(8) 0.0340(10) 0.0339(9) 0.0054(7) -0.0077(7) -0.0162(7) C13B 0.0215(9) 0.0364(11) 0.0589(15) 0.0003(10) 0.0063(9) -0.0095(8) C14B 0.0248(9) 0.0314(10) 0.0462(12) 0.0060(8) -0.0086(8) -0.0181(7) C15B 0.0451(14) 0.108(3) 0.0378(12) -0.0072(14) -0.0054(11) -0.0534(17) C16B 0.0186(7) 0.0177(7) 0.0148(6) -0.0025(5) -0.0020(5) -0.0048(5) C17B 0.0253(8) 0.0205(7) 0.0188(7) -0.0049(6) -0.0049(6) -0.0074(6) C18B 0.0286(9) 0.0248(8) 0.0154(7) -0.0054(6) -0.0050(6) -0.0036(6) C19B 0.0252(8) 0.0255(8) 0.0131(6) -0.0010(5) -0.0010(5) -0.0040(6) C20B 0.0204(7) 0.0235(8) 0.0169(7) -0.0001(6) -0.0009(5) -0.0072(6) C21B 0.0191(7) 0.0177(7) 0.0127(6) -0.0025(5) -0.0017(5) -0.0053(5) C22B 0.0183(7) 0.0181(7) 0.0148(6) -0.0017(5) -0.0006(5) -0.0071(5) C23B 0.0154(6) 0.0161(6) 0.0163(6) -0.0019(5) -0.0015(5) -0.0067(5) C24B 0.0154(6) 0.0166(6) 0.0178(6) -0.0022(5) 0.0001(5) -0.0069(5) C25B 0.0135(6) 0.0153(6) 0.0203(7) -0.0014(5) -0.0017(5) -0.0067(5) C26B 0.0153(6) 0.0170(7) 0.0178(6) -0.0030(5) -0.0024(5) -0.0064(5) C27B 0.0146(6) 0.0149(6) 0.0160(6) -0.0023(5) -0.0004(5) -0.0067(5) C28B 0.0142(6) 0.0162(6) 0.0168(6) -0.0019(5) -0.0015(5) -0.0067(5) C29B 0.0144(6) 0.0189(7) 0.0245(7) -0.0041(6) -0.0020(5) -0.0081(5) C30B 0.0170(7) 0.0360(10) 0.0319(9) -0.0067(7) 0.0030(6) -0.0137(7) C31B 0.0217(8) 0.0240(8) 0.0443(11) -0.0113(8) -0.0012(7) -0.0128(6) C32B 0.0208(8) 0.0316(9) 0.0320(9) 0.0019(7) -0.0094(7) -0.0107(7) C33B 0.0163(7) 0.0206(7) 0.0164(6) -0.0033(5) 0.0015(5) -0.0088(5) C34B 0.0238(8) 0.0294(9) 0.0184(7) -0.0070(6) 0.0007(6) -0.0116(6) C35B 0.0284(9) 0.0268(8) 0.0215(7) -0.0021(6) 0.0034(6) -0.0170(7) C36B 0.0170(7) 0.0253(8) 0.0262(8) -0.0078(6) 0.0003(6) -0.0063(6) N1S 0.0357(10) 0.0362(10) 0.0479(11) -0.0022(8) -0.0072(8) -0.0095(8) C1S 0.0291(9) 0.0250(9) 0.0324(9) -0.0026(7) 0.0019(7) -0.0099(7) C2S 0.0281(10) 0.0312(10) 0.0583(15) 0.0055(10) 0.0007(10) -0.0061(8) C1T 0.0528(15) 0.0398(12) 0.0400(13) 0.0066(10) 0.0061(11) -0.0101(11) N1T 0.115(3) 0.0666(18) 0.0394(13) -0.0018(12) 0.0182(15) -0.0258(17) C2T 0.089(2) 0.0344(13) 0.0501(16) -0.0064(11) -0.0117(15) -0.0122(14) C1R 0.074(2) 0.0426(14) 0.0306(12) -0.0098(10) -0.0020(12) 0.0062(14) N1R 0.115(3) 0.0526(16) 0.0430(14) -0.0074(11) 0.0136(15) -0.0184(17) C2R 0.0442(15) 0.0636(18) 0.0492(15) -0.0214(13) -0.0109(12) 0.0122(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1A C1A 1.3527(19) . ? C1A C6A 1.405(2) . ? C1A C2A 1.419(2) . ? N1A C7A 1.287(2) . ? N1A C16A 1.4214(19) . ? O2A C28A 1.3543(18) . ? C2A C3A 1.391(2) . ? C2A C8A 1.533(2) . ? N2A C22A 1.290(2) . ? N2A C21A 1.4190(19) . ? C3A C4A 1.404(2) . ? C4A C5A 1.387(2) . ? C4A C12A 1.532(2) . ? C5A C6A 1.408(2) . ? C6A C7A 1.457(2) . ? C8A C10A 1.536(2) . ? C8A C11A 1.537(2) . ? C8A C9A 1.539(3) . ? C12A C15A 1.530(2) . ? C12A C14A 1.537(2) . ? C12A C13A 1.541(2) . ? C16A C17A 1.399(2) . ? C16A C21A 1.411(2) . ? C17A C18A 1.393(2) . ? C18A C19A 1.392(2) . ? C19A C20A 1.399(2) . ? C20A C21A 1.399(2) . ? C22A C23A 1.452(2) . ? C23A C24A 1.405(2) . ? C23A C28A 1.413(2) . ? C24A C25A 1.380(2) . ? C25A C26A 1.411(2) . ? C25A C29A 1.530(2) . ? C26A C27A 1.394(2) . ? C27A C28A 1.414(2) . ? C27A C33A 1.537(2) . ? C29A C30A 1.533(3) . ? C29A C32A 1.534(2) . ? C29A C31A 1.537(2) . ? C33A C36A 1.530(2) . ? C33A C35A 1.536(2) . ? C33A C34A 1.542(2) . ? C1B O1B 1.3495(19) . ? C1B C6B 1.412(2) . ? C1B C2B 1.417(2) . ? N1B C7B 1.290(2) . ? N1B C16B 1.408(2) . ? C2B C3B 1.394(2) . ? C2B C8B 1.532(2) . ? O2B C28B 1.3500(19) . ? N2B C22B 1.292(2) . ? N2B C21B 1.409(2) . ? C3B C4B 1.404(2) . ? C4B C5B 1.389(2) . ? C4B C12B 1.537(2) . ? C5B C6B 1.407(2) . ? C6B C7B 1.452(2) . ? C8B C10B 1.532(2) . ? C8B C11B 1.538(2) . ? C8B C9B 1.544(2) . ? C12B C15B 1.500(3) . ? C12B C14B 1.534(3) . ? C12B C13B 1.559(3) . ? C16B C17B 1.396(2) . ? C16B C21B 1.402(2) . ? C17B C18B 1.393(2) . ? C18B C19B 1.382(3) . ? C19B C20B 1.388(2) . ? C20B C21B 1.398(2) . ? C22B C23B 1.445(2) . ? C23B C24B 1.404(2) . ? C23B C28B 1.417(2) . ? C24B C25B 1.380(2) . ? C25B C26B 1.412(2) . ? C25B C29B 1.531(2) . ? C26B C27B 1.394(2) . ? C27B C28B 1.412(2) . ? C27B C33B 1.536(2) . ? C29B C31B 1.532(2) . ? C29B C30B 1.534(2) . ? C29B C32B 1.543(2) . ? C33B C34B 1.530(2) . ? C33B C35B 1.540(2) . ? C33B C36B 1.543(2) . ? N1S C1S 1.140(3) . ? C1S C2S 1.456(3) . ? C1T N1T 1.143(4) . ? C1T C2T 1.452(4) . ? C1R N1R 1.161(5) . ? C1R C2R 1.455(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A C1A C6A 120.07(13) . . ? O1A C1A C2A 119.95(14) . . ? C6A C1A C2A 119.97(13) . . ? C7A N1A C16A 119.14(14) . . ? C3A C2A C1A 117.10(14) . . ? C3A C2A C8A 121.62(13) . . ? C1A C2A C8A 121.28(13) . . ? C22A N2A C21A 119.17(13) . . ? C2A C3A C4A 124.50(14) . . ? C5A C4A C3A 116.93(14) . . ? C5A C4A C12A 122.97(14) . . ? C3A C4A C12A 120.08(13) . . ? C4A C5A C6A 121.33(14) . . ? C1A C6A C5A 120.13(13) . . ? C1A C6A C7A 121.78(13) . . ? C5A C6A C7A 118.06(14) . . ? N1A C7A C6A 122.26(15) . . ? C2A C8A C10A 110.22(14) . . ? C2A C8A C11A 111.91(14) . . ? C10A C8A C11A 107.79(14) . . ? C2A C8A C9A 109.12(13) . . ? C10A C8A C9A 110.68(16) . . ? C11A C8A C9A 107.08(14) . . ? C15A C12A C4A 111.79(13) . . ? C15A C12A C14A 108.34(13) . . ? C4A C12A C14A 109.82(13) . . ? C15A C12A C13A 108.79(14) . . ? C4A C12A C13A 109.29(13) . . ? C14A C12A C13A 108.76(13) . . ? C17A C16A C21A 119.61(13) . . ? C17A C16A N1A 122.07(14) . . ? C21A C16A N1A 118.24(13) . . ? C18A C17A C16A 120.38(14) . . ? C19A C18A C17A 120.16(15) . . ? C18A C19A C20A 120.06(15) . . ? C19A C20A C21A 120.24(14) . . ? C20A C21A C16A 119.53(13) . . ? C20A C21A N2A 122.25(13) . . ? C16A C21A N2A 118.15(13) . . ? N2A C22A C23A 121.92(13) . . ? C24A C23A C28A 119.94(13) . . ? C24A C23A C22A 118.11(13) . . ? C28A C23A C22A 121.87(13) . . ? C25A C24A C23A 121.45(14) . . ? C24A C25A C26A 117.12(13) . . ? C24A C25A C29A 123.32(13) . . ? C26A C25A C29A 119.53(13) . . ? C27A C26A C25A 124.30(13) . . ? C26A C27A C28A 116.93(13) . . ? C26A C27A C33A 121.80(13) . . ? C28A C27A C33A 121.27(13) . . ? O2A C28A C23A 119.79(13) . . ? O2A C28A C27A 119.97(13) . . ? C23A C28A C27A 120.25(13) . . ? C25A C29A C30A 108.95(13) . . ? C25A C29A C32A 111.42(14) . . ? C30A C29A C32A 108.39(14) . . ? C25A C29A C31A 110.28(13) . . ? C30A C29A C31A 109.13(15) . . ? C32A C29A C31A 108.63(14) . . ? C36A C33A C35A 107.04(13) . . ? C36A C33A C27A 112.42(13) . . ? C35A C33A C27A 109.03(13) . . ? C36A C33A C34A 107.72(13) . . ? C35A C33A C34A 110.60(14) . . ? C27A C33A C34A 109.98(13) . . ? O1B C1B C6B 120.68(13) . . ? O1B C1B C2B 119.39(14) . . ? C6B C1B C2B 119.91(14) . . ? C7B N1B C16B 121.90(14) . . ? C3B C2B C1B 117.20(14) . . ? C3B C2B C8B 121.71(13) . . ? C1B C2B C8B 121.06(13) . . ? C22B N2B C21B 121.39(14) . . ? C2B C3B C4B 124.30(15) . . ? C5B C4B C3B 117.24(15) . . ? C5B C4B C12B 121.89(15) . . ? C3B C4B C12B 120.79(15) . . ? C4B C5B C6B 121.12(15) . . ? C5B C6B C1B 120.22(14) . . ? C5B C6B C7B 118.64(14) . . ? C1B C6B C7B 121.13(14) . . ? N1B C7B C6B 121.07(15) . . ? C2B C8B C10B 110.10(13) . . ? C2B C8B C11B 112.39(13) . . ? C10B C8B C11B 107.09(14) . . ? C2B C8B C9B 109.38(13) . . ? C10B C8B C9B 110.31(14) . . ? C11B C8B C9B 107.51(13) . . ? C15B C12B C14B 110.6(2) . . ? C15B C12B C4B 111.90(17) . . ? C14B C12B C4B 111.79(15) . . ? C15B C12B C13B 108.3(2) . . ? C14B C12B C13B 106.26(18) . . ? C4B C12B C13B 107.77(16) . . ? C17B C16B C21B 119.35(14) . . ? C17B C16B N1B 123.13(16) . . ? C21B C16B N1B 117.23(14) . . ? C18B C17B C16B 120.26(17) . . ? C19B C18B C17B 120.34(16) . . ? C18B C19B C20B 119.94(16) . . ? C19B C20B C21B 120.42(17) . . ? C20B C21B C16B 119.66(15) . . ? C20B C21B N2B 123.13(15) . . ? C16B C21B N2B 116.98(13) . . ? N2B C22B C23B 121.55(14) . . ? C24B C23B C28B 120.41(14) . . ? C24B C23B C22B 118.14(14) . . ? C28B C23B C22B 121.44(14) . . ? C25B C24B C23B 120.85(14) . . ? C24B C25B C26B 117.38(14) . . ? C24B C25B C29B 123.06(14) . . ? C26B C25B C29B 119.56(14) . . ? C27B C26B C25B 124.52(15) . . ? C26B C27B C28B 116.60(13) . . ? C26B C27B C33B 122.19(14) . . ? C28B C27B C33B 121.20(13) . . ? O2B C28B C27B 119.42(13) . . ? O2B C28B C23B 120.36(14) . . ? C27B C28B C23B 120.22(14) . . ? C25B C29B C31B 109.76(13) . . ? C25B C29B C30B 111.86(14) . . ? C31B C29B C30B 107.84(15) . . ? C25B C29B C32B 109.16(13) . . ? C31B C29B C32B 109.87(16) . . ? C30B C29B C32B 108.34(14) . . ? C34B C33B C27B 112.02(13) . . ? C34B C33B C35B 106.79(14) . . ? C27B C33B C35B 110.32(13) . . ? C34B C33B C36B 107.87(14) . . ? C27B C33B C36B 109.71(13) . . ? C35B C33B C36B 110.05(14) . . ? N1S C1S C2S 178.8(2) . . ? N1T C1T C2T 178.6(3) . . ? N1R C1R C2R 179.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A C1A C2A C3A 178.39(14) . . . . ? C6A C1A C2A C3A -2.0(2) . . . . ? O1A C1A C2A C8A -1.5(2) . . . . ? C6A C1A C2A C8A 178.15(14) . . . . ? C1A C2A C3A C4A 1.1(2) . . . . ? C8A C2A C3A C4A -179.09(14) . . . . ? C2A C3A C4A C5A 0.3(2) . . . . ? C2A C3A C4A C12A -178.15(14) . . . . ? C3A C4A C5A C6A -0.7(2) . . . . ? C12A C4A C5A C6A 177.67(14) . . . . ? O1A C1A C6A C5A -178.75(14) . . . . ? C2A C1A C6A C5A 1.6(2) . . . . ? O1A C1A C6A C7A -0.9(2) . . . . ? C2A C1A C6A C7A 179.53(14) . . . . ? C4A C5A C6A C1A -0.2(2) . . . . ? C4A C5A C6A C7A -178.19(14) . . . . ? C16A N1A C7A C6A 178.83(14) . . . . ? C1A C6A C7A N1A -2.6(2) . . . . ? C5A C6A C7A N1A 175.35(14) . . . . ? C3A C2A C8A C10A -118.46(17) . . . . ? C1A C2A C8A C10A 61.37(19) . . . . ? C3A C2A C8A C11A 1.5(2) . . . . ? C1A C2A C8A C11A -178.69(14) . . . . ? C3A C2A C8A C9A 119.80(17) . . . . ? C1A C2A C8A C9A -60.36(19) . . . . ? C5A C4A C12A C15A 8.3(2) . . . . ? C3A C4A C12A C15A -173.34(14) . . . . ? C5A C4A C12A C14A 128.58(15) . . . . ? C3A C4A C12A C14A -53.06(18) . . . . ? C5A C4A C12A C13A -112.19(17) . . . . ? C3A C4A C12A C13A 66.17(19) . . . . ? C7A N1A C16A C17A -43.4(2) . . . . ? C7A N1A C16A C21A 140.00(16) . . . . ? C21A C16A C17A C18A -1.3(3) . . . . ? N1A C16A C17A C18A -177.84(16) . . . . ? C16A C17A C18A C19A 0.1(3) . . . . ? C17A C18A C19A C20A 0.5(3) . . . . ? C18A C19A C20A C21A 0.0(3) . . . . ? C19A C20A C21A C16A -1.2(3) . . . . ? C19A C20A C21A N2A -178.28(16) . . . . ? C17A C16A C21A C20A 1.9(2) . . . . ? N1A C16A C21A C20A 178.53(15) . . . . ? C17A C16A C21A N2A 179.02(15) . . . . ? N1A C16A C21A N2A -4.3(2) . . . . ? C22A N2A C21A C20A -42.9(2) . . . . ? C22A N2A C21A C16A 139.98(16) . . . . ? C21A N2A C22A C23A -178.48(14) . . . . ? N2A C22A C23A C24A 174.06(15) . . . . ? N2A C22A C23A C28A -2.7(2) . . . . ? C28A C23A C24A C25A 0.1(2) . . . . ? C22A C23A C24A C25A -176.70(14) . . . . ? C23A C24A C25A C26A -0.9(2) . . . . ? C23A C24A C25A C29A 176.96(15) . . . . ? C24A C25A C26A C27A 0.4(2) . . . . ? C29A C25A C26A C27A -177.51(15) . . . . ? C25A C26A C27A C28A 0.8(2) . . . . ? C25A C26A C27A C33A -179.47(14) . . . . ? C24A C23A C28A O2A -178.81(14) . . . . ? C22A C23A C28A O2A -2.1(2) . . . . ? C24A C23A C28A C27A 1.1(2) . . . . ? C22A C23A C28A C27A 177.87(14) . . . . ? C26A C27A C28A O2A 178.40(14) . . . . ? C33A C27A C28A O2A -1.4(2) . . . . ? C26A C27A C28A C23A -1.6(2) . . . . ? C33A C27A C28A C23A 178.69(14) . . . . ? C24A C25A C29A C30A -110.54(18) . . . . ? C26A C25A C29A C30A 67.28(19) . . . . ? C24A C25A C29A C32A 9.0(2) . . . . ? C26A C25A C29A C32A -173.19(14) . . . . ? C24A C25A C29A C31A 129.71(17) . . . . ? C26A C25A C29A C31A -52.5(2) . . . . ? C26A C27A C33A C36A 1.3(2) . . . . ? C28A C27A C33A C36A -178.95(14) . . . . ? C26A C27A C33A C35A 119.85(16) . . . . ? C28A C27A C33A C35A -60.41(19) . . . . ? C26A C27A C33A C34A -118.72(16) . . . . ? C28A C27A C33A C34A 61.02(19) . . . . ? O1B C1B C2B C3B 179.65(15) . . . . ? C6B C1B C2B C3B 0.6(2) . . . . ? O1B C1B C2B C8B 1.3(2) . . . . ? C6B C1B C2B C8B -177.76(14) . . . . ? C1B C2B C3B C4B -0.3(2) . . . . ? C8B C2B C3B C4B 178.03(16) . . . . ? C2B C3B C4B C5B -0.1(3) . . . . ? C2B C3B C4B C12B 176.79(16) . . . . ? C3B C4B C5B C6B 0.2(2) . . . . ? C12B C4B C5B C6B -176.62(16) . . . . ? C4B C5B C6B C1B 0.1(2) . . . . ? C4B C5B C6B C7B -178.45(15) . . . . ? O1B C1B C6B C5B -179.52(15) . . . . ? C2B C1B C6B C5B -0.5(2) . . . . ? O1B C1B C6B C7B -1.0(2) . . . . ? C2B C1B C6B C7B 177.99(15) . . . . ? C16B N1B C7B C6B -176.11(14) . . . . ? C5B C6B C7B N1B -179.79(15) . . . . ? C1B C6B C7B N1B 1.7(2) . . . . ? C3B C2B C8B C10B 121.71(17) . . . . ? C1B C2B C8B C10B -60.00(19) . . . . ? C3B C2B C8B C11B 2.4(2) . . . . ? C1B C2B C8B C11B -179.29(15) . . . . ? C3B C2B C8B C9B -116.92(17) . . . . ? C1B C2B C8B C9B 61.37(19) . . . . ? C5B C4B C12B C15B -31.6(3) . . . . ? C3B C4B C12B C15B 151.7(2) . . . . ? C5B C4B C12B C14B -156.23(18) . . . . ? C3B C4B C12B C14B 27.0(3) . . . . ? C5B C4B C12B C13B 87.4(2) . . . . ? C3B C4B C12B C13B -89.4(2) . . . . ? C7B N1B C16B C17B 39.5(2) . . . . ? C7B N1B C16B C21B -146.74(16) . . . . ? C21B C16B C17B C18B 1.1(2) . . . . ? N1B C16B C17B C18B 174.80(15) . . . . ? C16B C17B C18B C19B -0.1(3) . . . . ? C17B C18B C19B C20B -0.1(3) . . . . ? C18B C19B C20B C21B -0.7(3) . . . . ? C19B C20B C21B C16B 1.7(2) . . . . ? C19B C20B C21B N2B 176.03(15) . . . . ? C17B C16B C21B C20B -1.9(2) . . . . ? N1B C16B C21B C20B -175.93(14) . . . . ? C17B C16B C21B N2B -176.59(14) . . . . ? N1B C16B C21B N2B 9.4(2) . . . . ? C22B N2B C21B C20B 35.0(2) . . . . ? C22B N2B C21B C16B -150.46(15) . . . . ? C21B N2B C22B C23B -175.41(14) . . . . ? N2B C22B C23B C24B -179.85(14) . . . . ? N2B C22B C23B C28B 0.7(2) . . . . ? C28B C23B C24B C25B 0.1(2) . . . . ? C22B C23B C24B C25B -179.34(14) . . . . ? C23B C24B C25B C26B -0.5(2) . . . . ? C23B C24B C25B C29B -179.64(14) . . . . ? C24B C25B C26B C27B 0.4(2) . . . . ? C29B C25B C26B C27B 179.59(14) . . . . ? C25B C26B C27B C28B 0.1(2) . . . . ? C25B C26B C27B C33B -179.57(14) . . . . ? C26B C27B C28B O2B 179.52(13) . . . . ? C33B C27B C28B O2B -0.8(2) . . . . ? C26B C27B C28B C23B -0.5(2) . . . . ? C33B C27B C28B C23B 179.14(14) . . . . ? C24B C23B C28B O2B -179.59(14) . . . . ? C22B C23B C28B O2B -0.2(2) . . . . ? C24B C23B C28B C27B 0.5(2) . . . . ? C22B C23B C28B C27B 179.86(14) . . . . ? C24B C25B C29B C31B -124.09(17) . . . . ? C26B C25B C29B C31B 56.79(19) . . . . ? C24B C25B C29B C30B -4.4(2) . . . . ? C26B C25B C29B C30B 176.44(15) . . . . ? C24B C25B C29B C32B 115.45(17) . . . . ? C26B C25B C29B C32B -63.67(19) . . . . ? C26B C27B C33B C34B 1.7(2) . . . . ? C28B C27B C33B C34B -177.92(14) . . . . ? C26B C27B C33B C35B 120.55(16) . . . . ? C28B C27B C33B C35B -59.10(19) . . . . ? C26B C27B C33B C36B -118.05(16) . . . . ? C28B C27B C33B C36B 62.31(19) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 35.18 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.954 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.068